Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Matilde Fondo' _publ_contact_author_address ; Departmento de Quimica Inorganica Universidad de Santiago de Compostela Facutade de Cienceas Lugo 27002 SPAIN ; _publ_contact_author_email QIMATF69@USC.ES _publ_section_title ; Dinuclear nickel complexes with a Ni2O2 core: a structural and magnetic study ; loop_ _publ_author_name 'Matilde Fondo' 'Manuel Bermejo' 'Ana M.Garcia-Deibe' 'Antonio Llamas-Saiz' 'Noelia Ocampo' ; J.Sanmartin ; #END data_4.3MeOH _database_code_depnum_ccdc_archive 'CCDC 291778' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H31 Br3 N4 Ni2 O8, 3(C H4 O)' _chemical_formula_sum 'C38 H43 Br3 N4 Ni2 O11' _chemical_formula_weight 1088.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.6463(16) _cell_length_b 10.6223(10) _cell_length_c 23.150(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.273(2) _cell_angle_gamma 90.00 _cell_volume 4027.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1379 _cell_measurement_theta_min 2.285 _cell_measurement_theta_max 24.565 _exptl_crystal_description neddle _exptl_crystal_colour green _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.796 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2192 _exptl_absorpt_coefficient_mu 3.976 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3914 _exptl_absorpt_correction_T_max 0.8571 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6184 _diffrn_reflns_av_R_equivalents 0.0579 _diffrn_reflns_av_sigmaI/netI 0.1120 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 23.32 _reflns_number_total 5811 _reflns_number_gt 3414 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER Smart' _computing_cell_refinement 'BRUKER Smart' _computing_data_reduction ? _computing_structure_solution 'SIR-92 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'Wingx 1.70.01 (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5811 _refine_ls_number_parameters 525 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1052 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.1125 _refine_ls_wR_factor_gt 0.0983 _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_restrained_S_all 0.950 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni11 Ni 0.52895(6) 0.24229(9) 0.22522(4) 0.0091(2) Uani 1 1 d . . . Ni12 Ni 0.59247(6) -0.01458(9) 0.27409(4) 0.0104(3) Uani 1 1 d . . . O101 O 0.4733(3) 0.3062(5) 0.2885(2) 0.0116(13) Uani 1 1 d . . . O102 O 0.5379(3) -0.0449(5) 0.3471(2) 0.0121(13) Uani 1 1 d . . . O103 O 0.4846(3) 0.0663(5) 0.2376(2) 0.0119(13) Uani 1 1 d . . . N101 N 0.4421(4) 0.3171(6) 0.1644(3) 0.0086(15) Uani 1 1 d . . . N102 N 0.5748(4) -0.2011(6) 0.2615(3) 0.0109(15) Uani 1 1 d . . . N103 N 0.5751(3) 0.1701(5) 0.1502(3) 0.0072(15) Uani 1 1 d . . . N104 N 0.6264(4) -0.0191(6) 0.1886(3) 0.0116(15) Uani 1 1 d . . . O10 O 0.6216(3) 0.1721(5) 0.2901(2) 0.0107(12) Uani 1 1 d . . . O12 O 0.7107(3) -0.0533(5) 0.3108(2) 0.0136(13) Uani 1 1 d . . . O1W O 0.5924(3) 0.4151(5) 0.2295(2) 0.0114(13) Uani 1 1 d . . . C100 C 0.4290(4) 0.4093(7) 0.2847(3) 0.0104(19) Uani 1 1 d . . . C101 C 0.4149(4) 0.4663(8) 0.3366(3) 0.015(2) Uani 1 1 d . . . H101 H 0.4385 0.4312 0.3735 0.018 Uiso 1 1 calc R . . C102 C 0.3665(5) 0.5746(7) 0.3346(4) 0.014(2) Uani 1 1 d . . . H102 H 0.3578 0.6124 0.3702 0.017 Uiso 1 1 calc R . . C103 C 0.3313(5) 0.6266(7) 0.2818(4) 0.015(2) Uani 1 1 d . . . Br11 Br 0.26152(5) 0.76782(8) 0.28227(4) 0.0239(2) Uani 1 1 d . . . C104 C 0.3446(4) 0.5744(7) 0.2307(4) 0.013(2) Uani 1 1 d . . . H104 H 0.3211 0.6120 0.1944 0.016 Uiso 1 1 calc R . . C105 C 0.3932(4) 0.4643(7) 0.2309(3) 0.0122(19) Uani 1 1 d . . . C106 C 0.4000(5) 0.4126(8) 0.1733(4) 0.016(2) Uani 1 1 d . . . H106 H 0.3704 0.4541 0.1397 0.019 Uiso 1 1 calc R . . C107 C 0.4439(5) 0.2729(8) 0.1039(3) 0.016(2) Uani 1 1 d . . . H10A H 0.4210 0.3382 0.0751 0.020 Uiso 1 1 calc R . . H10B H 0.4109 0.1954 0.0955 0.020 Uiso 1 1 calc R . . C108 C 0.5325(4) 0.2466(8) 0.0994(3) 0.0142(19) Uani 1 1 d . . . H10C H 0.5344 0.2009 0.0624 0.017 Uiso 1 1 calc R . . H10D H 0.5617 0.3275 0.0980 0.017 Uiso 1 1 calc R . . C109 C 0.6665(4) 0.1812(7) 0.1561(3) 0.0083(18) Uani 1 1 d . . . H10E H 0.6872 0.2544 0.1808 0.010 Uiso 1 1 calc R . . H10F H 0.6824 0.1910 0.1171 0.010 Uiso 1 1 calc R . . C110 C 0.7001(4) 0.0587(7) 0.1850(3) 0.014(2) Uani 1 1 d . . . H11A H 0.7356 0.0159 0.1611 0.016 Uiso 1 1 calc R . . H11B H 0.7320 0.0747 0.2247 0.016 Uiso 1 1 calc R . . C111 C 0.6428(4) -0.1554(6) 0.1798(3) 0.0087(18) Uani 1 1 d . . . H11C H 0.6984 -0.1762 0.2008 0.010 Uiso 1 1 calc R . . H11D H 0.6410 -0.1715 0.1375 0.010 Uiso 1 1 calc R . . C112 C 0.5815(5) -0.2406(7) 0.2020(3) 0.0120(18) Uani 1 1 d . . . H11E H 0.5277 -0.2342 0.1758 0.014 Uiso 1 1 calc R . . H11F H 0.6000 -0.3292 0.2022 0.014 Uiso 1 1 calc R . . C113 C 0.5743(4) -0.2846(7) 0.3002(3) 0.0130(19) Uani 1 1 d . . . H113 H 0.5754 -0.3700 0.2882 0.016 Uiso 1 1 calc R . . C114 C 0.5721(4) -0.2607(7) 0.3625(3) 0.0069(17) Uani 1 1 d . . . C115 C 0.5889(5) -0.3621(8) 0.4021(4) 0.018(2) Uani 1 1 d . . . H115 H 0.6026 -0.4419 0.3881 0.022 Uiso 1 1 calc R . . C116 C 0.5857(5) -0.3473(8) 0.4605(4) 0.020(2) Uani 1 1 d . . . Br12 Br 0.61270(5) -0.48444(8) 0.51168(4) 0.0242(2) Uani 1 1 d . . . C117 C 0.5609(5) -0.2335(7) 0.4809(4) 0.018(2) Uani 1 1 d . . . H117 H 0.5558 -0.2246 0.5209 0.022 Uiso 1 1 calc R . . C118 C 0.5437(5) -0.1330(7) 0.4426(3) 0.0139(19) Uani 1 1 d . . . H118 H 0.5265 -0.0553 0.4567 0.017 Uiso 1 1 calc R . . C119 C 0.5511(4) -0.1438(7) 0.3842(3) 0.0102(18) Uani 1 1 d . . . C120 C 0.5627(5) 0.0337(7) 0.1406(3) 0.0140(19) Uani 1 1 d . . . H120 H 0.5780 0.0115 0.1020 0.017 Uiso 1 1 calc R . . C121 C 0.4772(4) -0.0132(7) 0.1408(3) 0.0126(19) Uani 1 1 d . . . C122 C 0.4365(5) -0.0776(7) 0.0929(4) 0.017(2) Uani 1 1 d . . . H122 H 0.4614 -0.0929 0.0597 0.021 Uiso 1 1 calc R . . C123 C 0.3570(5) -0.1200(8) 0.0946(4) 0.025(2) Uani 1 1 d . . . Br13 Br 0.30057(5) -0.21752(10) 0.03127(5) 0.0388(3) Uani 1 1 d . . . C124 C 0.3215(5) -0.0970(8) 0.1426(4) 0.022(2) Uani 1 1 d . . . H124 H 0.2674 -0.1253 0.1426 0.026 Uiso 1 1 calc R . . C125 C 0.3624(5) -0.0341(8) 0.1904(4) 0.019(2) Uani 1 1 d . . . H125 H 0.3370 -0.0199 0.2235 0.023 Uiso 1 1 calc R . . C126 C 0.4422(4) 0.0095(7) 0.1905(3) 0.0123(19) Uani 1 1 d . . . C10 C 0.6481(4) 0.2324(8) 0.3374(3) 0.0104(18) Uani 1 1 d . . . O11 O 0.6573(3) 0.3487(5) 0.3391(2) 0.0119(13) Uani 1 1 d . . . C11 C 0.6679(4) 0.1636(7) 0.3944(3) 0.0126(19) Uani 1 1 d . . . C12 C 0.6393(5) 0.2098(8) 0.4432(4) 0.018(2) Uani 1 1 d . . . H12 H 0.6049 0.2818 0.4387 0.022 Uiso 1 1 calc R . . C13 C 0.6590(5) 0.1551(8) 0.4978(3) 0.016(2) Uani 1 1 d . . . H13 H 0.6359 0.1858 0.5297 0.020 Uiso 1 1 calc R . . C14 C 0.7125(5) 0.0553(8) 0.5054(4) 0.022(2) Uani 1 1 d . . . H14 H 0.7281 0.0185 0.5432 0.027 Uiso 1 1 calc R . . C15 C 0.7439(5) 0.0082(7) 0.4578(3) 0.0150(19) Uani 1 1 d . . . H15 H 0.7817 -0.0595 0.4637 0.018 Uiso 1 1 calc R . . C16 C 0.7212(4) 0.0576(7) 0.4021(3) 0.0111(19) Uani 1 1 d . . . C17 C 0.7570(5) -0.0018(7) 0.3532(3) 0.0108(19) Uani 1 1 d . . . O13 O 0.8338(3) 0.0000(5) 0.3588(2) 0.0146(13) Uani 1 1 d . . . H2 H 0.5039 0.0304 0.3532 0.050 Uiso 1 1 d . . . H1W1 H 0.6314 0.4177 0.2701 0.050 Uiso 1 1 d . . . H1W2 H 0.6223 0.4294 0.2009 0.050 Uiso 1 1 d . . . O1S O 0.4558(3) 0.1426(5) 0.3704(2) 0.0153(13) Uani 1 1 d . . . H1S H 0.4634 0.2109 0.3539 0.023 Uiso 1 1 calc R . . C1S C 0.3704(5) 0.1093(8) 0.3567(4) 0.026(2) Uani 1 1 d . . . H1S1 H 0.3629 0.0237 0.3707 0.039 Uiso 1 1 calc R . . H1S2 H 0.3518 0.1130 0.3141 0.039 Uiso 1 1 calc R . . H1S3 H 0.3386 0.1685 0.3761 0.039 Uiso 1 1 calc R . . O2S O 0.5969(3) 0.8655(6) 0.0212(3) 0.0332(17) Uani 1 1 d . . . H2S H 0.5873 0.7901 0.0286 0.050 Uiso 1 1 calc R . . C2S C 0.6801(5) 0.8794(9) 0.0188(4) 0.040(3) Uani 1 1 d . . . H2S1 H 0.6872 0.9488 -0.0078 0.060 Uiso 1 1 calc R . . H2S2 H 0.7008 0.8013 0.0043 0.060 Uiso 1 1 calc R . . H2S3 H 0.7105 0.8979 0.0581 0.060 Uiso 1 1 calc R . . O3S O 0.5708(4) 0.6227(6) 0.0525(3) 0.052(2) Uani 1 1 d . . . H3S H 0.6045 0.5865 0.0786 0.078 Uiso 1 1 calc R . . C3S C 0.4943(6) 0.5980(9) 0.0610(5) 0.042(3) Uani 1 1 d . . . H3S1 H 0.4961 0.5654 0.1008 0.063 Uiso 1 1 calc R . . H3S2 H 0.4692 0.5351 0.0324 0.063 Uiso 1 1 calc R . . H3S3 H 0.4619 0.6755 0.0559 0.063 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni11 0.0071(5) 0.0104(6) 0.0102(5) 0.0005(5) 0.0022(4) 0.0003(5) Ni12 0.0083(6) 0.0125(6) 0.0110(6) -0.0011(5) 0.0032(4) 0.0015(5) O101 0.008(3) 0.016(3) 0.013(3) 0.002(2) 0.007(2) 0.006(2) O102 0.016(3) 0.006(3) 0.015(3) 0.005(3) 0.006(3) 0.005(2) O103 0.010(3) 0.018(3) 0.007(3) -0.001(2) 0.000(2) 0.000(2) N101 0.005(4) 0.006(4) 0.014(4) 0.000(3) 0.001(3) -0.004(3) N102 0.009(4) 0.012(4) 0.011(4) -0.003(3) 0.001(3) 0.003(3) N103 0.009(3) 0.009(3) 0.022(4) 0.001(3) 0.007(3) 0.001(3) N104 0.016(4) 0.004(4) 0.013(4) 0.000(3) 0.000(3) -0.002(3) O10 0.008(3) 0.014(3) 0.014(3) -0.005(3) -0.003(2) 0.007(2) O12 0.013(3) 0.015(3) 0.012(3) -0.003(3) 0.001(3) 0.005(3) O1W 0.008(3) 0.014(3) 0.013(3) 0.000(2) 0.004(2) 0.003(2) C100 0.009(4) 0.012(5) 0.018(5) 0.005(4) -0.001(4) -0.007(4) C101 0.010(5) 0.027(5) 0.009(5) 0.003(4) 0.004(4) -0.003(4) C102 0.017(5) 0.011(5) 0.019(5) 0.002(4) 0.015(4) 0.005(4) C103 0.012(5) 0.010(5) 0.024(5) 0.005(4) 0.003(4) 0.001(4) Br11 0.0240(5) 0.0197(5) 0.0313(6) 0.0017(4) 0.0139(4) 0.0112(4) C104 0.005(5) 0.010(5) 0.022(5) 0.007(4) -0.002(4) 0.003(4) C105 0.009(4) 0.015(5) 0.021(5) -0.005(4) 0.000(4) -0.009(4) C106 0.008(5) 0.020(5) 0.023(5) 0.008(4) -0.005(4) -0.006(4) C107 0.011(5) 0.023(5) 0.014(5) -0.005(4) -0.002(4) -0.005(4) C108 0.012(4) 0.024(5) 0.008(4) 0.006(4) 0.006(3) 0.003(4) C109 0.007(4) 0.011(4) 0.007(4) 0.003(4) 0.001(3) 0.001(3) C110 0.008(5) 0.020(5) 0.013(5) 0.006(4) 0.002(4) -0.003(4) C111 0.009(4) 0.009(4) 0.011(5) -0.001(4) 0.004(4) 0.004(4) C112 0.021(5) 0.015(5) 0.007(4) -0.001(4) 0.002(3) 0.004(4) C113 0.016(5) 0.008(5) 0.016(5) -0.004(4) 0.007(4) 0.003(4) C114 0.006(4) 0.013(5) 0.007(4) -0.001(4) -0.003(3) -0.005(4) C115 0.019(5) 0.020(5) 0.015(5) -0.005(4) 0.002(4) 0.002(4) C116 0.012(5) 0.023(6) 0.025(6) 0.013(4) 0.004(4) 0.007(4) Br12 0.0344(6) 0.0198(5) 0.0194(5) 0.0063(4) 0.0073(4) 0.0054(4) C117 0.018(5) 0.015(5) 0.022(5) -0.005(4) 0.008(4) 0.000(4) C118 0.019(5) 0.010(5) 0.014(5) 0.000(4) 0.005(4) 0.002(4) C119 0.005(4) 0.017(5) 0.007(5) -0.004(4) -0.003(4) 0.000(4) C120 0.012(5) 0.018(5) 0.011(5) 0.000(4) -0.001(4) 0.005(4) C121 0.012(5) 0.015(5) 0.013(5) 0.001(4) 0.006(4) -0.006(4) C122 0.012(5) 0.020(5) 0.020(5) -0.005(4) 0.004(4) -0.004(4) C123 0.024(6) 0.021(5) 0.026(6) -0.010(4) -0.007(5) -0.001(4) Br13 0.0184(5) 0.0495(7) 0.0449(7) -0.0308(6) -0.0040(5) -0.0046(5) C124 0.012(5) 0.027(6) 0.026(6) -0.009(5) 0.006(4) -0.007(4) C125 0.006(5) 0.025(5) 0.027(5) -0.002(4) 0.005(4) -0.001(4) C126 0.011(5) 0.013(5) 0.009(5) 0.003(4) -0.005(4) 0.000(4) C10 0.004(4) 0.018(5) 0.009(5) 0.001(4) 0.000(4) 0.006(4) O11 0.008(3) 0.011(3) 0.014(3) -0.003(3) -0.007(2) -0.001(2) C11 0.002(4) 0.022(5) 0.014(5) -0.006(4) 0.001(4) 0.000(4) C12 0.011(5) 0.015(5) 0.027(5) -0.008(4) 0.004(4) 0.003(4) C13 0.024(5) 0.020(5) 0.007(5) -0.007(4) 0.006(4) -0.003(4) C14 0.025(6) 0.031(6) 0.012(5) 0.008(4) 0.004(4) -0.006(5) C15 0.020(5) 0.015(5) 0.012(5) 0.008(4) 0.009(4) 0.002(4) C16 0.007(4) 0.010(5) 0.018(5) 0.000(4) 0.008(4) -0.001(4) C17 0.016(5) 0.003(4) 0.013(5) 0.002(4) 0.002(4) 0.001(4) O13 0.006(3) 0.016(3) 0.022(3) -0.003(3) 0.005(2) 0.003(3) O1S 0.017(3) 0.009(3) 0.020(4) 0.003(3) 0.005(3) 0.003(2) C1S 0.016(5) 0.035(6) 0.028(6) 0.017(5) 0.007(4) 0.001(4) O2S 0.017(4) 0.054(5) 0.028(4) -0.001(4) 0.000(3) 0.005(3) C2S 0.029(6) 0.059(8) 0.026(6) 0.007(5) -0.009(5) 0.005(6) O3S 0.026(4) 0.064(5) 0.066(6) 0.034(4) 0.006(4) -0.002(4) C3S 0.039(7) 0.024(6) 0.060(8) 0.003(5) 0.003(6) 0.005(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni11 O101 1.987(5) . ? Ni11 N101 1.994(6) . ? Ni11 O103 2.049(5) . ? Ni11 O10 2.089(5) . ? Ni11 O1W 2.111(5) . ? Ni11 N103 2.162(6) . ? Ni12 N102 2.017(6) . ? Ni12 O103 2.033(5) . ? Ni12 O12 2.042(5) . ? Ni12 O10 2.059(5) . ? Ni12 O102 2.082(5) . ? Ni12 N104 2.154(6) . ? O101 C100 1.315(8) . ? O102 C119 1.349(9) . ? O102 H2 1.0051 . ? O103 C126 1.333(8) . ? N101 C106 1.271(9) . ? N101 C107 1.483(9) . ? N102 C113 1.262(9) . ? N102 C112 1.464(9) . ? N103 C120 1.475(9) . ? N103 C108 1.500(9) . ? N103 C109 1.507(9) . ? N104 C110 1.492(9) . ? N104 C111 1.494(9) . ? N104 C120 1.501(9) . ? O10 C10 1.279(9) . ? O12 C17 1.261(9) . ? O1W H1W1 1.0439 . ? O1W H1W2 0.9084 . ? C100 C101 1.402(10) . ? C100 C105 1.407(10) . ? C101 C102 1.400(10) . ? C101 H101 0.9500 . ? C102 C103 1.375(11) . ? C102 H102 0.9500 . ? C103 C104 1.359(11) . ? C103 Br11 1.898(8) . ? C104 C105 1.421(10) . ? C104 H104 0.9500 . ? C105 C106 1.466(11) . ? C106 H106 0.9500 . ? C107 C108 1.522(10) . ? C107 H10A 0.9900 . ? C107 H10B 0.9900 . ? C108 H10C 0.9900 . ? C108 H10D 0.9900 . ? C109 C110 1.524(10) . ? C109 H10E 0.9900 . ? C109 H10F 0.9900 . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 C112 1.519(9) . ? C111 H11C 0.9900 . ? C111 H11D 0.9900 . ? C112 H11E 0.9900 . ? C112 H11F 0.9900 . ? C113 C114 1.470(10) . ? C113 H113 0.9500 . ? C114 C119 1.407(10) . ? C114 C115 1.410(10) . ? C115 C116 1.371(11) . ? C115 H115 0.9500 . ? C116 C117 1.386(11) . ? C116 Br12 1.881(8) . ? C117 C118 1.384(10) . ? C117 H117 0.9500 . ? C118 C119 1.385(10) . ? C118 H118 0.9500 . ? C120 C121 1.510(10) . ? C120 H120 1.0000 . ? C121 C122 1.373(10) . ? C121 C126 1.399(10) . ? C122 C123 1.406(11) . ? C122 H122 0.9500 . ? C123 C124 1.370(11) . ? C123 Br13 1.901(8) . ? C124 C125 1.365(11) . ? C124 H124 0.9500 . ? C125 C126 1.408(10) . ? C125 H125 0.9500 . ? C10 O11 1.244(9) . ? C10 C11 1.491(10) . ? C11 C12 1.393(10) . ? C11 C16 1.425(10) . ? C12 C13 1.376(11) . ? C12 H12 0.9500 . ? C13 C14 1.376(11) . ? C13 H13 0.9500 . ? C14 C15 1.395(10) . ? C14 H14 0.9500 . ? C15 C16 1.380(10) . ? C15 H15 0.9500 . ? C16 C17 1.508(10) . ? C17 O13 1.262(8) . ? O1S C1S 1.445(9) . ? O1S H1S 0.8400 . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? O2S C2S 1.404(9) . ? O2S H2S 0.8400 . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? O3S C3S 1.348(10) . ? O3S H3S 0.8400 . ? C3S H3S1 0.9800 . ? C3S H3S2 0.9800 . ? C3S H3S3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O101 Ni11 N101 90.6(2) . . ? O101 Ni11 O103 89.0(2) . . ? N101 Ni11 O103 103.2(2) . . ? O101 Ni11 O10 88.5(2) . . ? N101 Ni11 O10 177.5(2) . . ? O103 Ni11 O10 79.1(2) . . ? O101 Ni11 O1W 87.9(2) . . ? N101 Ni11 O1W 88.9(2) . . ? O103 Ni11 O1W 167.6(2) . . ? O10 Ni11 O1W 88.73(19) . . ? O101 Ni11 N103 173.2(2) . . ? N101 Ni11 N103 83.7(2) . . ? O103 Ni11 N103 88.7(2) . . ? O10 Ni11 N103 97.4(2) . . ? O1W Ni11 N103 95.7(2) . . ? N102 Ni12 O103 105.0(2) . . ? N102 Ni12 O12 88.1(2) . . ? O103 Ni12 O12 166.5(2) . . ? N102 Ni12 O10 174.7(2) . . ? O103 Ni12 O10 80.2(2) . . ? O12 Ni12 O10 86.6(2) . . ? N102 Ni12 O102 83.8(2) . . ? O103 Ni12 O102 85.55(19) . . ? O12 Ni12 O102 99.1(2) . . ? O10 Ni12 O102 97.2(2) . . ? N102 Ni12 N104 84.3(2) . . ? O103 Ni12 N104 89.1(2) . . ? O12 Ni12 N104 89.2(2) . . ? O10 Ni12 N104 95.4(2) . . ? O102 Ni12 N104 165.2(2) . . ? C100 O101 Ni11 124.4(5) . . ? C119 O102 Ni12 126.3(4) . . ? C119 O102 H2 124.2 . . ? Ni12 O102 H2 109.2 . . ? C126 O103 Ni12 116.6(4) . . ? C126 O103 Ni11 116.7(4) . . ? Ni12 O103 Ni11 97.5(2) . . ? C106 N101 C107 120.7(7) . . ? C106 N101 Ni11 123.7(6) . . ? C107 N101 Ni11 114.0(5) . . ? C113 N102 C112 118.6(6) . . ? C113 N102 Ni12 127.4(5) . . ? C112 N102 Ni12 112.5(5) . . ? C120 N103 C108 112.4(6) . . ? C120 N103 C109 101.7(5) . . ? C108 N103 C109 110.9(5) . . ? C120 N103 Ni11 114.2(4) . . ? C108 N103 Ni11 104.6(4) . . ? C109 N103 Ni11 113.4(4) . . ? C110 N104 C111 111.0(6) . . ? C110 N104 C120 103.3(5) . . ? C111 N104 C120 112.5(6) . . ? C110 N104 Ni12 113.0(4) . . ? C111 N104 Ni12 103.3(4) . . ? C120 N104 Ni12 113.9(4) . . ? C10 O10 Ni12 132.2(5) . . ? C10 O10 Ni11 122.4(4) . . ? Ni12 O10 Ni11 95.4(2) . . ? C17 O12 Ni12 130.3(5) . . ? Ni11 O1W H1W1 106.9 . . ? Ni11 O1W H1W2 116.5 . . ? H1W1 O1W H1W2 108.5 . . ? O101 C100 C101 118.7(7) . . ? O101 C100 C105 123.3(7) . . ? C101 C100 C105 118.0(7) . . ? C102 C101 C100 120.7(7) . . ? C102 C101 H101 119.7 . . ? C100 C101 H101 119.7 . . ? C103 C102 C101 120.7(7) . . ? C103 C102 H102 119.6 . . ? C101 C102 H102 119.6 . . ? C104 C103 C102 120.0(7) . . ? C104 C103 Br11 121.5(6) . . ? C102 C103 Br11 118.5(6) . . ? C103 C104 C105 120.9(8) . . ? C103 C104 H104 119.5 . . ? C105 C104 H104 119.5 . . ? C100 C105 C104 119.7(7) . . ? C100 C105 C106 124.1(7) . . ? C104 C105 C106 116.2(7) . . ? N101 C106 C105 125.5(8) . . ? N101 C106 H106 117.3 . . ? C105 C106 H106 117.3 . . ? N101 C107 C108 107.8(6) . . ? N101 C107 H10A 110.1 . . ? C108 C107 H10A 110.1 . . ? N101 C107 H10B 110.1 . . ? C108 C107 H10B 110.1 . . ? H10A C107 H10B 108.5 . . ? N103 C108 C107 112.0(6) . . ? N103 C108 H10C 109.2 . . ? C107 C108 H10C 109.2 . . ? N103 C108 H10D 109.2 . . ? C107 C108 H10D 109.2 . . ? H10C C108 H10D 107.9 . . ? N103 C109 C110 104.9(6) . . ? N103 C109 H10E 110.8 . . ? C110 C109 H10E 110.8 . . ? N103 C109 H10F 110.8 . . ? C110 C109 H10F 110.8 . . ? H10E C109 H10F 108.8 . . ? N104 C110 C109 104.9(6) . . ? N104 C110 H11A 110.8 . . ? C109 C110 H11A 110.8 . . ? N104 C110 H11B 110.8 . . ? C109 C110 H11B 110.8 . . ? H11A C110 H11B 108.8 . . ? N104 C111 C112 112.4(6) . . ? N104 C111 H11C 109.1 . . ? C112 C111 H11C 109.1 . . ? N104 C111 H11D 109.1 . . ? C112 C111 H11D 109.1 . . ? H11C C111 H11D 107.8 . . ? N102 C112 C111 108.4(6) . . ? N102 C112 H11E 110.0 . . ? C111 C112 H11E 110.0 . . ? N102 C112 H11F 110.0 . . ? C111 C112 H11F 110.0 . . ? H11E C112 H11F 108.4 . . ? N102 C113 C114 125.4(7) . . ? N102 C113 H113 117.3 . . ? C114 C113 H113 117.3 . . ? C119 C114 C115 118.3(7) . . ? C119 C114 C113 123.7(7) . . ? C115 C114 C113 118.0(7) . . ? C116 C115 C114 121.0(8) . . ? C116 C115 H115 119.5 . . ? C114 C115 H115 119.5 . . ? C115 C116 C117 120.1(8) . . ? C115 C116 Br12 119.0(6) . . ? C117 C116 Br12 120.8(6) . . ? C118 C117 C116 119.6(8) . . ? C118 C117 H117 120.2 . . ? C116 C117 H117 120.2 . . ? C117 C118 C119 121.1(7) . . ? C117 C118 H118 119.4 . . ? C119 C118 H118 119.4 . . ? O102 C119 C118 121.7(7) . . ? O102 C119 C114 118.8(6) . . ? C118 C119 C114 119.5(7) . . ? N103 C120 N104 101.2(6) . . ? N103 C120 C121 115.5(6) . . ? N104 C120 C121 114.6(6) . . ? N103 C120 H120 108.4 . . ? N104 C120 H120 108.4 . . ? C121 C120 H120 108.4 . . ? C122 C121 C126 122.1(7) . . ? C122 C121 C120 119.4(7) . . ? C126 C121 C120 118.4(7) . . ? C121 C122 C123 117.9(7) . . ? C121 C122 H122 121.0 . . ? C123 C122 H122 121.0 . . ? C124 C123 C122 120.6(8) . . ? C124 C123 Br13 119.9(7) . . ? C122 C123 Br13 119.5(6) . . ? C125 C124 C123 121.3(8) . . ? C125 C124 H124 119.3 . . ? C123 C124 H124 119.3 . . ? C124 C125 C126 119.7(7) . . ? C124 C125 H125 120.1 . . ? C126 C125 H125 120.1 . . ? O103 C126 C121 120.9(7) . . ? O103 C126 C125 120.8(7) . . ? C121 C126 C125 118.2(7) . . ? O11 C10 O10 123.1(7) . . ? O11 C10 C11 116.9(7) . . ? O10 C10 C11 120.0(7) . . ? C12 C11 C16 118.1(7) . . ? C12 C11 C10 119.4(7) . . ? C16 C11 C10 122.2(7) . . ? C13 C12 C11 122.5(8) . . ? C13 C12 H12 118.8 . . ? C11 C12 H12 118.8 . . ? C12 C13 C14 119.1(7) . . ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4 . . ? C13 C14 C15 120.0(8) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C16 C15 C14 121.6(8) . . ? C16 C15 H15 119.2 . . ? C14 C15 H15 119.2 . . ? C15 C16 C11 118.6(7) . . ? C15 C16 C17 117.6(7) . . ? C11 C16 C17 123.8(7) . . ? O12 C17 O13 123.6(7) . . ? O12 C17 C16 119.8(7) . . ? O13 C17 C16 116.5(7) . . ? C1S O1S H1S 109.5 . . ? O1S C1S H1S1 109.5 . . ? O1S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? O1S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? C2S O2S H2S 109.5 . . ? O2S C2S H2S1 109.5 . . ? O2S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? O2S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? C3S O3S H3S 109.5 . . ? O3S C3S H3S1 109.5 . . ? O3S C3S H3S2 109.5 . . ? H3S1 C3S H3S2 109.5 . . ? O3S C3S H3S3 109.5 . . ? H3S1 C3S H3S3 109.5 . . ? H3S2 C3S H3S3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N101 Ni11 O101 C100 -30.3(6) . . . . ? O103 Ni11 O101 C100 -133.5(5) . . . . ? O10 Ni11 O101 C100 147.3(6) . . . . ? O1W Ni11 O101 C100 58.6(6) . . . . ? N102 Ni12 O102 C119 40.9(6) . . . . ? O103 Ni12 O102 C119 146.6(6) . . . . ? O12 Ni12 O102 C119 -46.2(6) . . . . ? O10 Ni12 O102 C119 -133.9(6) . . . . ? N102 Ni12 O103 C126 -33.3(5) . . . . ? O12 Ni12 O103 C126 133.5(8) . . . . ? O10 Ni12 O103 C126 146.2(5) . . . . ? O102 Ni12 O103 C126 -115.6(5) . . . . ? N104 Ni12 O103 C126 50.6(5) . . . . ? N102 Ni12 O103 Ni11 -158.3(2) . . . . ? O10 Ni12 O103 Ni11 21.25(19) . . . . ? O102 Ni12 O103 Ni11 119.4(2) . . . . ? N104 Ni12 O103 Ni11 -74.4(2) . . . . ? O101 Ni11 O103 C126 125.4(5) . . . . ? N101 Ni11 O103 C126 35.1(5) . . . . ? O10 Ni11 O103 C126 -145.9(5) . . . . ? O1W Ni11 O103 C126 -159.0(8) . . . . ? N103 Ni11 O103 C126 -48.2(5) . . . . ? O101 Ni11 O103 Ni12 -109.6(2) . . . . ? N101 Ni11 O103 Ni12 160.0(2) . . . . ? O10 Ni11 O103 Ni12 -21.01(19) . . . . ? N103 Ni11 O103 Ni12 76.8(2) . . . . ? O101 Ni11 N101 C106 27.1(6) . . . . ? O103 Ni11 N101 C106 116.1(6) . . . . ? O1W Ni11 N101 C106 -60.8(6) . . . . ? N103 Ni11 N101 C106 -156.7(6) . . . . ? O101 Ni11 N101 C107 -167.4(5) . . . . ? O103 Ni11 N101 C107 -78.3(5) . . . . ? O1W Ni11 N101 C107 104.7(5) . . . . ? N103 Ni11 N101 C107 8.9(5) . . . . ? O103 Ni12 N102 C113 -114.5(6) . . . . ? O12 Ni12 N102 C113 68.6(7) . . . . ? O102 Ni12 N102 C113 -30.8(6) . . . . ? N104 Ni12 N102 C113 158.0(7) . . . . ? O103 Ni12 N102 C112 79.7(5) . . . . ? O12 Ni12 N102 C112 -97.2(5) . . . . ? O102 Ni12 N102 C112 163.4(5) . . . . ? N104 Ni12 N102 C112 -7.8(5) . . . . ? N101 Ni11 N103 C120 -107.0(5) . . . . ? O103 Ni11 N103 C120 -3.6(5) . . . . ? O10 Ni11 N103 C120 75.3(5) . . . . ? O1W Ni11 N103 C120 164.8(5) . . . . ? N101 Ni11 N103 C108 16.2(4) . . . . ? O103 Ni11 N103 C108 119.6(4) . . . . ? O10 Ni11 N103 C108 -161.5(4) . . . . ? O1W Ni11 N103 C108 -72.1(4) . . . . ? N101 Ni11 N103 C109 137.2(5) . . . . ? O103 Ni11 N103 C109 -119.4(4) . . . . ? O10 Ni11 N103 C109 -40.5(5) . . . . ? O1W Ni11 N103 C109 48.9(5) . . . . ? N102 Ni12 N104 C110 -137.5(5) . . . . ? O103 Ni12 N104 C110 117.3(5) . . . . ? O12 Ni12 N104 C110 -49.3(5) . . . . ? O10 Ni12 N104 C110 37.2(5) . . . . ? O102 Ni12 N104 C110 -174.0(7) . . . . ? N102 Ni12 N104 C111 -17.5(4) . . . . ? O103 Ni12 N104 C111 -122.7(4) . . . . ? O12 Ni12 N104 C111 70.7(4) . . . . ? O10 Ni12 N104 C111 157.2(4) . . . . ? N102 Ni12 N104 C120 104.9(5) . . . . ? O103 Ni12 N104 C120 -0.3(5) . . . . ? O12 Ni12 N104 C120 -166.9(5) . . . . ? O10 Ni12 N104 C120 -80.3(5) . . . . ? O103 Ni12 O10 C10 123.5(6) . . . . ? O12 Ni12 O10 C10 -59.4(6) . . . . ? O102 Ni12 O10 C10 39.3(6) . . . . ? N104 Ni12 O10 C10 -148.3(6) . . . . ? O103 Ni12 O10 Ni11 -20.74(18) . . . . ? O12 Ni12 O10 Ni11 156.3(2) . . . . ? O102 Ni12 O10 Ni11 -104.9(2) . . . . ? N104 Ni12 O10 Ni11 67.4(2) . . . . ? O101 Ni11 O10 C10 -39.3(5) . . . . ? O103 Ni11 O10 C10 -128.5(6) . . . . ? O1W Ni11 O10 C10 48.7(5) . . . . ? N103 Ni11 O10 C10 144.2(5) . . . . ? O101 Ni11 O10 Ni12 109.9(2) . . . . ? O103 Ni11 O10 Ni12 20.65(18) . . . . ? O1W Ni11 O10 Ni12 -162.2(2) . . . . ? N103 Ni11 O10 Ni12 -66.6(2) . . . . ? N102 Ni12 O12 C17 -143.6(6) . . . . ? O10 Ni12 O12 C17 36.6(6) . . . . ? O102 Ni12 O12 C17 -60.2(6) . . . . ? N104 Ni12 O12 C17 132.1(6) . . . . ? Ni11 O101 C100 C101 -159.8(5) . . . . ? Ni11 O101 C100 C105 21.7(9) . . . . ? O101 C100 C101 C102 -178.5(7) . . . . ? C101 C102 C103 Br11 176.6(6) . . . . ? C102 C103 C104 C105 1.5(12) . . . . ? Br11 C103 C104 C105 -176.3(5) . . . . ? O101 C100 C105 C104 178.6(7) . . . . ? C101 C100 C105 C106 -177.7(7) . . . . ? C103 C104 C105 C106 177.0(7) . . . . ? C107 N101 C106 C105 179.7(7) . . . . ? C104 C105 C106 N101 178.1(7) . . . . ? C106 N101 C107 C108 134.1(7) . . . . ? Ni11 N101 C107 C108 -31.9(7) . . . . ? C120 N103 C108 C107 85.8(8) . . . . ? C109 N103 C108 C107 -161.2(6) . . . . ? Ni11 N103 C108 C107 -38.6(7) . . . . ? N101 C107 C108 N103 47.4(8) . . . . ? C120 N103 C109 C110 -32.9(7) . . . . ? C108 N103 C109 C110 -152.5(6) . . . . ? Ni11 N103 C109 C110 90.1(6) . . . . ? C111 N104 C110 C109 144.8(6) . . . . ? C120 N104 C110 C109 24.0(7) . . . . ? Ni12 N104 C110 C109 -99.6(6) . . . . ? N103 C109 C110 N104 5.2(7) . . . . ? C110 N104 C111 C112 161.6(6) . . . . ? C120 N104 C111 C112 -83.1(7) . . . . ? Ni12 N104 C111 C112 40.2(7) . . . . ? C113 N102 C112 C111 -135.7(7) . . . . ? Ni12 N102 C112 C111 31.5(7) . . . . ? N104 C111 C112 N102 -49.2(8) . . . . ? C112 N102 C113 C114 176.7(7) . . . . ? N102 C113 C114 C115 -167.1(7) . . . . ? C113 C114 C115 C116 -178.2(7) . . . . ? C114 C115 C116 Br12 -177.6(6) . . . . ? Br12 C116 C117 C118 178.2(6) . . . . ? Ni12 O102 C119 C118 150.5(6) . . . . ? Ni12 O102 C119 C114 -30.0(9) . . . . ? C117 C118 C119 O102 -177.0(7) . . . . ? C115 C114 C119 O102 177.5(6) . . . . ? C113 C114 C119 C118 174.3(7) . . . . ? C108 N103 C120 N104 166.5(5) . . . . ? C109 N103 C120 N104 47.8(6) . . . . ? Ni11 N103 C120 N104 -74.7(6) . . . . ? C108 N103 C120 C121 -69.2(8) . . . . ? C109 N103 C120 C121 172.2(6) . . . . ? Ni11 N103 C120 C121 49.7(7) . . . . ? C110 N104 C120 N103 -45.0(7) . . . . ? C111 N104 C120 N103 -164.8(5) . . . . ? Ni12 N104 C120 N103 78.0(6) . . . . ? C110 N104 C120 C121 -170.0(6) . . . . ? C111 N104 C120 C121 70.2(8) . . . . ? Ni12 N104 C120 C121 -47.0(7) . . . . ? N103 C120 C121 C122 123.6(8) . . . . ? N104 C120 C121 C122 -119.3(8) . . . . ? N104 C120 C121 C126 59.9(9) . . . . ? C120 C121 C122 C123 179.9(7) . . . . ? C121 C122 C123 Br13 -176.6(6) . . . . ? Br13 C123 C124 C125 175.8(6) . . . . ? Ni12 O103 C126 C121 -56.2(9) . . . . ? Ni11 O103 C126 C121 58.4(8) . . . . ? Ni12 O103 C126 C125 121.0(7) . . . . ? Ni11 O103 C126 C125 -124.4(7) . . . . ? C122 C121 C126 O103 176.3(7) . . . . ? C120 C121 C126 C125 179.9(7) . . . . ? C124 C125 C126 O103 -177.1(7) . . . . ? Ni12 O10 C10 O11 -175.0(5) . . . . ? Ni11 O10 C10 O11 -38.5(9) . . . . ? Ni11 O10 C10 C11 140.1(5) . . . . ? O10 C10 C11 C12 -132.7(8) . . . . ? O11 C10 C11 C16 -128.5(8) . . . . ? C10 C11 C12 C13 -176.3(7) . . . . ? C14 C15 C16 C17 -178.6(7) . . . . ? C10 C11 C16 C15 172.6(7) . . . . ? C12 C11 C16 C17 -179.7(7) . . . . ? Ni12 O12 C17 O13 -152.9(5) . . . . ? C15 C16 C17 O12 117.9(8) . . . . ? C11 C16 C17 O13 118.0(8) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O102 H2 O1S 1.01 1.53 2.527(7) 173.1 . O1W H1W1 O11 1.04 1.74 2.670(7) 145.9 . O1W H1W2 O13 0.91 1.83 2.719(7) 163.7 2_655 O1S H1S O101 0.84 1.85 2.626(7) 152.3 . O2S H2S O3S 0.84 1.90 2.735(9) 174.7 . O3S H3S O13 0.84 1.86 2.697(8) 171.8 2_655 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 23.32 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.091 _refine_diff_density_min -1.003 _refine_diff_density_rms 0.150 data_1.H2O _database_code_depnum_ccdc_archive 'CCDC 606600' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H38 N4 Ni2 O6, H2 O' _chemical_formula_sum 'C33 H40 N4 Ni2 O7' _chemical_formula_weight 722.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.569(3) _cell_length_b 20.834(5) _cell_length_c 14.508(3) _cell_angle_alpha 90.00 _cell_angle_beta 112.486(3) _cell_angle_gamma 90.00 _cell_volume 3231.0(12) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1472 _cell_measurement_theta_min 2.855 _cell_measurement_theta_max 25.92 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 1.219 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7310 _exptl_absorpt_correction_T_max 0.9304 _exptl_absorpt_process_details 'SADABS-2004/1 (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart-CCD-1000 BRUKER' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.1 _diffrn_reflns_number 52423 _diffrn_reflns_av_R_equivalents 0.0503 _diffrn_reflns_av_sigmaI/netI 0.0556 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 26.50 _reflns_number_total 6682 _reflns_number_gt 4685 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER Smart' _computing_cell_refinement 'BRUKER Smart' _computing_data_reduction ? _computing_structure_solution 'SIR92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0480P)^2^+0.6538P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6682 _refine_ls_number_parameters 429 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0668 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.0988 _refine_ls_wR_factor_gt 0.0904 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni11 Ni 0.98594(3) 0.132528(18) 0.63946(3) 0.01175(10) Uani 1 1 d . . . Ni12 Ni 0.87562(3) 0.269102(18) 0.61432(3) 0.01170(10) Uani 1 1 d . . . O101 O 1.05264(18) 0.11541(9) 0.78604(14) 0.0159(5) Uani 1 1 d . . . O102 O 0.90776(19) 0.30160(10) 0.75126(14) 0.0170(5) Uani 1 1 d . . . O103 O 1.04954(17) 0.22679(9) 0.65822(13) 0.0117(4) Uani 1 1 d . . . N101 N 1.1303(2) 0.08374(11) 0.63005(17) 0.0129(5) Uani 1 1 d . . . N102 N 0.9174(2) 0.35439(12) 0.57222(18) 0.0156(6) Uani 1 1 d . . . N103 N 0.9317(2) 0.14259(11) 0.48048(18) 0.0138(5) Uani 1 1 d . . . N104 N 0.8452(2) 0.24339(11) 0.46150(16) 0.0114(5) Uani 1 1 d . . . O10 O 0.83210(18) 0.17640(9) 0.64496(13) 0.0135(4) Uani 1 1 d . . . O11 O 0.89144(18) 0.04637(9) 0.61964(14) 0.0156(5) Uani 1 1 d . . . O12S O 0.6834(2) 0.29774(10) 0.56703(16) 0.0175(5) Uani 1 1 d . . . C10 C 0.6801(3) 0.19173(16) 0.7165(2) 0.0221(7) Uani 1 1 d . . . H10A H 0.6923 0.2366 0.7020 0.033 Uiso 0.12(3) 1 calc PR . . H10B H 0.7015 0.1866 0.7883 0.033 Uiso 0.12(3) 1 calc PR . . H10C H 0.5924 0.1797 0.6801 0.033 Uiso 0.12(3) 1 calc PR . . H10D H 0.6318 0.1653 0.7449 0.033 Uiso 0.88(3) 1 calc PR . . H10E H 0.6227 0.2153 0.6586 0.033 Uiso 0.88(3) 1 calc PR . . H10F H 0.7317 0.2222 0.7668 0.033 Uiso 0.88(3) 1 calc PR . . C11 C 0.7623(3) 0.14962(14) 0.6847(2) 0.0147(6) Uani 1 1 d . . . C12 C 0.7585(3) 0.08382(15) 0.6992(2) 0.0178(7) Uani 1 1 d . . . H12 H 0.7077 0.0694 0.7333 0.021 Uiso 1 1 calc R . . C13 C 0.8231(3) 0.03615(15) 0.6679(2) 0.0157(7) Uani 1 1 d . . . C14 C 0.8105(3) -0.03225(15) 0.6961(2) 0.0242(7) Uani 1 1 d . . . H14A H 0.8591 -0.0604 0.6702 0.036 Uiso 0.14(3) 1 calc PR . . H14B H 0.7223 -0.0449 0.6674 0.036 Uiso 0.14(3) 1 calc PR . . H14C H 0.8420 -0.0360 0.7689 0.036 Uiso 0.14(3) 1 calc PR . . H14D H 0.7565 -0.0338 0.7341 0.036 Uiso 0.86(3) 1 calc PR . . H14E H 0.8933 -0.0493 0.7369 0.036 Uiso 0.86(3) 1 calc PR . . H14F H 0.7736 -0.0582 0.6355 0.036 Uiso 0.86(3) 1 calc PR . . C12S C 0.6467(3) 0.34775(15) 0.6171(2) 0.0200(7) Uani 1 1 d . . . H12A H 0.5561 0.3541 0.5853 0.030 Uiso 1 1 calc R . . H12B H 0.6897 0.3876 0.6132 0.030 Uiso 1 1 calc R . . H12C H 0.6691 0.3359 0.6872 0.030 Uiso 1 1 calc R . . C100 C 1.1118(3) 0.06324(14) 0.8285(2) 0.0151(6) Uani 1 1 d . . . C101 C 1.1085(3) 0.04239(15) 0.9198(2) 0.0215(7) Uani 1 1 d . . . H101 H 1.0597 0.0657 0.9482 0.026 Uiso 1 1 calc R . . C102 C 1.1735(3) -0.01043(16) 0.9688(2) 0.0262(8) Uani 1 1 d . . . H102 H 1.1703 -0.0225 1.0310 0.031 Uiso 1 1 calc R . . C103 C 1.2442(3) -0.04666(16) 0.9289(2) 0.0275(8) Uani 1 1 d . . . H103 H 1.2896 -0.0832 0.9633 0.033 Uiso 1 1 calc R . . C104 C 1.2469(3) -0.02838(15) 0.8385(2) 0.0223(7) Uani 1 1 d . . . H104 H 1.2944 -0.0532 0.8106 0.027 Uiso 1 1 calc R . . C105 C 1.1820(3) 0.02562(14) 0.7860(2) 0.0162(7) Uani 1 1 d . . . C106 C 1.1889(3) 0.03935(14) 0.6909(2) 0.0161(7) Uani 1 1 d . . . H106 H 1.2424 0.0128 0.6714 0.019 Uiso 1 1 calc R . . C107 C 1.1397(3) 0.08758(15) 0.5332(2) 0.0170(7) Uani 1 1 d . . . H10G H 1.1809 0.0486 0.5212 0.020 Uiso 1 1 calc R . . H10H H 1.1898 0.1255 0.5304 0.020 Uiso 1 1 calc R . . C108 C 1.0072(3) 0.09319(15) 0.4546(2) 0.0162(7) Uani 1 1 d . . . H10I H 1.0116 0.1043 0.3897 0.019 Uiso 1 1 calc R . . H10J H 0.9649 0.0511 0.4472 0.019 Uiso 1 1 calc R . . C109 C 0.7961(3) 0.13237(14) 0.4227(2) 0.0166(7) Uani 1 1 d . . . H10K H 0.7616 0.1006 0.4562 0.020 Uiso 1 1 calc R . . H10L H 0.7808 0.1171 0.3544 0.020 Uiso 1 1 calc R . . C110 C 0.7379(3) 0.19800(14) 0.4199(2) 0.0145(6) Uani 1 1 d . . . H11A H 0.6843 0.2099 0.3507 0.017 Uiso 1 1 calc R . . H11B H 0.6864 0.1983 0.4610 0.017 Uiso 1 1 calc R . . C111 C 0.8187(3) 0.30601(14) 0.4086(2) 0.0151(6) Uani 1 1 d . . . H11C H 0.7314 0.3188 0.3956 0.018 Uiso 1 1 calc R . . H11D H 0.8268 0.3013 0.3435 0.018 Uiso 1 1 calc R . . C112 C 0.9070(3) 0.35818(15) 0.4686(2) 0.0181(7) Uani 1 1 d . . . H11E H 0.9904 0.3524 0.4655 0.022 Uiso 1 1 calc R . . H11F H 0.8745 0.4008 0.4405 0.022 Uiso 1 1 calc R . . C113 C 0.9446(3) 0.40595(15) 0.6245(2) 0.0162(7) Uani 1 1 d . . . H113 H 0.9524 0.4443 0.5919 0.019 Uiso 1 1 calc R . . C114 C 0.9643(3) 0.41042(15) 0.7288(2) 0.0175(7) Uani 1 1 d . . . C115 C 1.0050(3) 0.47053(16) 0.7735(2) 0.0228(7) Uani 1 1 d . . . H115 H 1.0134 0.5049 0.7335 0.027 Uiso 1 1 calc R . . C116 C 1.0330(3) 0.48113(17) 0.8734(3) 0.0285(8) Uani 1 1 d . . . H116 H 1.0618 0.5219 0.9024 0.034 Uiso 1 1 calc R . . C117 C 1.0181(3) 0.43077(18) 0.9309(2) 0.0275(8) Uani 1 1 d . . . H117 H 1.0391 0.4368 1.0003 0.033 Uiso 1 1 calc R . . C118 C 0.9729(3) 0.37208(16) 0.8877(2) 0.0215(7) Uani 1 1 d . . . H118 H 0.9592 0.3393 0.9279 0.026 Uiso 1 1 calc R . . C119 C 0.9465(3) 0.35887(15) 0.7862(2) 0.0184(7) Uani 1 1 d . . . C120 C 0.9502(3) 0.20807(14) 0.4492(2) 0.0133(6) Uani 1 1 d . . . H120 H 0.9350 0.2070 0.3765 0.016 Uiso 1 1 calc R . . C121 C 1.0776(3) 0.23512(14) 0.5045(2) 0.0138(6) Uani 1 1 d . . . C122 C 1.1530(3) 0.25098(14) 0.4535(2) 0.0164(7) Uani 1 1 d . . . H122 H 1.1222 0.2448 0.3834 0.020 Uiso 1 1 calc R . . C123 C 1.2724(3) 0.27564(15) 0.5019(2) 0.0221(7) Uani 1 1 d . . . H123 H 1.3244 0.2853 0.4665 0.026 Uiso 1 1 calc R . . C124 C 1.3130(3) 0.28571(16) 0.6039(2) 0.0232(8) Uani 1 1 d . . . H124 H 1.3941 0.3030 0.6389 0.028 Uiso 1 1 calc R . . C125 C 1.2378(3) 0.27115(15) 0.6558(2) 0.0188(7) Uani 1 1 d . . . H125 H 1.2673 0.2798 0.7253 0.023 Uiso 1 1 calc R . . C126 C 1.1198(3) 0.24403(13) 0.6080(2) 0.0128(6) Uani 1 1 d . . . H12S H 0.632(3) 0.2921(16) 0.515(3) 0.024(10) Uiso 1 1 d . . . O1W O 0.9942(2) 0.20387(14) 0.89303(16) 0.0183(5) Uani 1 1 d . . . H1W1 H 1.008(3) 0.1758(18) 0.859(3) 0.026(11) Uiso 1 1 d . . . H2W1 H 0.976(3) 0.2326(18) 0.862(3) 0.026(12) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni11 0.0127(2) 0.0120(2) 0.01060(19) -0.00073(15) 0.00449(15) 0.00020(15) Ni12 0.0132(2) 0.0123(2) 0.00862(18) -0.00080(15) 0.00303(14) 0.00073(15) O101 0.0176(11) 0.0153(11) 0.0130(10) -0.0003(8) 0.0039(9) 0.0025(9) O102 0.0233(12) 0.0153(12) 0.0107(10) -0.0030(8) 0.0045(9) 0.0020(9) O103 0.0113(10) 0.0128(11) 0.0108(10) -0.0011(8) 0.0038(8) -0.0003(8) N101 0.0104(12) 0.0169(14) 0.0106(12) -0.0023(10) 0.0031(10) -0.0011(10) N102 0.0134(13) 0.0179(15) 0.0136(13) -0.0012(10) 0.0029(10) 0.0005(10) N103 0.0115(13) 0.0149(14) 0.0155(13) -0.0028(10) 0.0056(10) 0.0000(10) N104 0.0116(12) 0.0111(13) 0.0101(12) 0.0000(9) 0.0024(10) 0.0001(10) O10 0.0134(10) 0.0151(11) 0.0116(10) 0.0018(8) 0.0045(8) 0.0010(9) O11 0.0179(11) 0.0143(11) 0.0168(11) -0.0011(8) 0.0092(9) -0.0010(9) O12S 0.0143(11) 0.0218(12) 0.0122(11) -0.0031(9) 0.0005(9) 0.0027(9) C10 0.0233(18) 0.0232(19) 0.0231(17) 0.0027(14) 0.0126(14) 0.0025(14) C11 0.0125(15) 0.0190(17) 0.0101(14) -0.0024(12) 0.0016(12) -0.0033(12) C12 0.0169(16) 0.0234(18) 0.0154(15) -0.0004(13) 0.0089(13) -0.0045(13) C13 0.0143(16) 0.0185(17) 0.0118(15) -0.0010(12) 0.0022(12) -0.0023(13) C14 0.0261(18) 0.0223(19) 0.0281(19) 0.0017(14) 0.0149(15) -0.0028(15) C12S 0.0220(17) 0.0207(18) 0.0167(16) -0.0025(13) 0.0067(13) 0.0033(14) C100 0.0135(15) 0.0136(16) 0.0140(15) -0.0026(12) 0.0007(12) -0.0048(12) C101 0.0266(18) 0.0200(18) 0.0185(16) -0.0010(13) 0.0095(14) -0.0020(14) C102 0.034(2) 0.0254(19) 0.0147(16) 0.0047(14) 0.0043(14) 0.0001(16) C103 0.034(2) 0.0192(19) 0.0237(18) 0.0064(14) 0.0043(15) 0.0060(15) C104 0.0229(18) 0.0162(17) 0.0238(18) -0.0002(13) 0.0042(14) 0.0035(14) C105 0.0150(15) 0.0163(16) 0.0136(15) -0.0004(12) 0.0012(12) -0.0007(13) C106 0.0119(15) 0.0159(17) 0.0173(15) -0.0063(12) 0.0021(12) 0.0019(12) C107 0.0185(16) 0.0197(17) 0.0149(15) -0.0009(12) 0.0086(13) 0.0013(13) C108 0.0195(16) 0.0174(17) 0.0143(15) -0.0041(12) 0.0093(13) 0.0011(13) C109 0.0158(16) 0.0160(16) 0.0158(15) -0.0053(13) 0.0036(12) -0.0017(13) C110 0.0092(15) 0.0180(17) 0.0146(15) -0.0031(12) 0.0026(12) -0.0038(12) C111 0.0164(16) 0.0149(16) 0.0117(15) -0.0007(12) 0.0027(12) 0.0022(13) C112 0.0183(16) 0.0186(17) 0.0151(15) 0.0025(12) 0.0038(13) 0.0001(13) C113 0.0134(15) 0.0142(17) 0.0182(16) -0.0032(12) 0.0029(12) -0.0007(12) C114 0.0113(15) 0.0199(18) 0.0199(16) -0.0055(13) 0.0046(12) 0.0037(13) C115 0.0186(17) 0.0194(18) 0.0297(19) -0.0092(14) 0.0086(14) -0.0022(14) C116 0.0191(18) 0.029(2) 0.036(2) -0.0200(16) 0.0088(15) -0.0013(15) C117 0.0146(17) 0.045(2) 0.0190(17) -0.0142(16) 0.0017(13) 0.0069(15) C118 0.0181(17) 0.028(2) 0.0151(16) -0.0015(14) 0.0032(13) 0.0092(14) C119 0.0086(15) 0.0242(19) 0.0179(16) -0.0046(13) 0.0002(12) 0.0069(13) C120 0.0133(15) 0.0195(16) 0.0068(14) -0.0007(11) 0.0036(11) -0.0001(12) C121 0.0147(15) 0.0121(16) 0.0130(15) 0.0022(12) 0.0037(12) 0.0040(12) C122 0.0180(16) 0.0194(17) 0.0118(14) 0.0012(12) 0.0056(12) 0.0006(13) C123 0.0215(17) 0.0260(19) 0.0234(17) 0.0039(14) 0.0140(14) -0.0016(14) C124 0.0154(17) 0.030(2) 0.0204(17) -0.0022(14) 0.0028(13) -0.0067(14) C125 0.0192(16) 0.0199(17) 0.0130(15) -0.0003(13) 0.0015(12) -0.0028(13) C126 0.0144(15) 0.0089(15) 0.0166(15) 0.0045(11) 0.0075(12) 0.0047(12) O1W 0.0213(12) 0.0201(14) 0.0118(11) 0.0002(11) 0.0046(9) 0.0038(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni11 O101 1.997(2) . ? Ni11 N101 2.004(2) . ? Ni11 O10 2.029(2) . ? Ni11 O11 2.064(2) . ? Ni11 O103 2.078(2) . ? Ni11 N103 2.157(2) . ? Ni12 O102 1.995(2) . ? Ni12 N102 1.998(3) . ? Ni12 O103 2.0618(19) . ? Ni12 O10 2.086(2) . ? Ni12 O12S 2.146(2) . ? Ni12 N104 2.175(2) . ? O101 C100 1.307(3) . ? O102 C119 1.307(4) . ? O103 C126 1.332(3) . ? N101 C106 1.279(4) . ? N101 C107 1.452(4) . ? N102 C113 1.282(4) . ? N102 C112 1.464(4) . ? N103 C120 1.479(4) . ? N103 C109 1.485(4) . ? N103 C108 1.488(4) . ? N104 C111 1.485(4) . ? N104 C120 1.489(4) . ? N104 C110 1.492(3) . ? O10 C11 1.285(3) . ? O11 C13 1.258(3) . ? O12S C12S 1.424(3) . ? O12S H12S 0.77(3) . ? C10 C11 1.491(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C10 H10D 0.9800 . ? C10 H10E 0.9800 . ? C10 H10F 0.9800 . ? C11 C12 1.390(4) . ? C12 C13 1.418(4) . ? C12 H12 0.9500 . ? C13 C14 1.505(4) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C14 H14D 0.9800 . ? C14 H14E 0.9800 . ? C14 H14F 0.9800 . ? C12S H12A 0.9800 . ? C12S H12B 0.9800 . ? C12S H12C 0.9800 . ? C100 C101 1.408(4) . ? C100 C105 1.427(4) . ? C101 C102 1.369(4) . ? C101 H101 0.9500 . ? C102 C103 1.391(5) . ? C102 H102 0.9500 . ? C103 C104 1.378(4) . ? C103 H103 0.9500 . ? C104 C105 1.404(4) . ? C104 H104 0.9500 . ? C105 C106 1.441(4) . ? C106 H106 0.9500 . ? C107 C108 1.525(4) . ? C107 H10G 0.9900 . ? C107 H10H 0.9900 . ? C108 H10I 0.9900 . ? C108 H10J 0.9900 . ? C109 C110 1.518(4) . ? C109 H10K 0.9900 . ? C109 H10L 0.9900 . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 C112 1.517(4) . ? C111 H11C 0.9900 . ? C111 H11D 0.9900 . ? C112 H11E 0.9900 . ? C112 H11F 0.9900 . ? C113 C114 1.444(4) . ? C113 H113 0.9500 . ? C114 C115 1.406(4) . ? C114 C119 1.422(4) . ? C115 C116 1.376(4) . ? C115 H115 0.9500 . ? C116 C117 1.391(5) . ? C116 H116 0.9500 . ? C117 C118 1.382(5) . ? C117 H117 0.9500 . ? C118 C119 1.412(4) . ? C118 H118 0.9500 . ? C120 C121 1.493(4) . ? C120 H120 1.0000 . ? C121 C122 1.382(4) . ? C121 C126 1.402(4) . ? C122 C123 1.387(4) . ? C122 H122 0.9500 . ? C123 C124 1.387(4) . ? C123 H123 0.9500 . ? C124 C125 1.384(4) . ? C124 H124 0.9500 . ? C125 C126 1.393(4) . ? C125 H125 0.9500 . ? O1W H1W1 0.82(4) . ? O1W H2W1 0.73(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O101 Ni11 N101 89.38(9) . . ? O101 Ni11 O10 91.50(8) . . ? N101 Ni11 O10 175.95(9) . . ? O101 Ni11 O11 87.79(8) . . ? N101 Ni11 O11 87.72(9) . . ? O10 Ni11 O11 88.36(8) . . ? O101 Ni11 O103 93.21(8) . . ? N101 Ni11 O103 103.05(9) . . ? O10 Ni11 O103 80.86(8) . . ? O11 Ni11 O103 169.19(8) . . ? O101 Ni11 N103 172.72(9) . . ? N101 Ni11 N103 83.43(9) . . ? O10 Ni11 N103 95.60(8) . . ? O11 Ni11 N103 90.78(8) . . ? O103 Ni11 N103 89.53(8) . . ? O102 Ni12 N102 91.60(9) . . ? O102 Ni12 O103 92.83(8) . . ? N102 Ni12 O103 98.81(9) . . ? O102 Ni12 O10 94.03(8) . . ? N102 Ni12 O10 174.28(9) . . ? O103 Ni12 O10 79.92(8) . . ? O102 Ni12 O12S 89.98(8) . . ? N102 Ni12 O12S 89.84(9) . . ? O103 Ni12 O12S 170.82(8) . . ? O10 Ni12 O12S 91.17(8) . . ? O102 Ni12 N104 174.19(9) . . ? N102 Ni12 N104 82.60(9) . . ? O103 Ni12 N104 88.16(8) . . ? O10 Ni12 N104 91.78(8) . . ? O12S Ni12 N104 89.93(8) . . ? C100 O101 Ni11 124.76(18) . . ? C119 O102 Ni12 126.99(19) . . ? C126 O103 Ni12 116.32(16) . . ? C126 O103 Ni11 116.28(17) . . ? Ni12 O103 Ni11 96.24(8) . . ? C106 N101 C107 119.4(3) . . ? C106 N101 Ni11 123.8(2) . . ? C107 N101 Ni11 114.25(18) . . ? C113 N102 C112 117.8(3) . . ? C113 N102 Ni12 126.7(2) . . ? C112 N102 Ni12 115.31(18) . . ? C120 N103 C109 101.8(2) . . ? C120 N103 C108 113.1(2) . . ? C109 N103 C108 110.7(2) . . ? C120 N103 Ni11 113.66(17) . . ? C109 N103 Ni11 113.70(18) . . ? C108 N103 Ni11 104.11(17) . . ? C111 N104 C120 112.9(2) . . ? C111 N104 C110 111.9(2) . . ? C120 N104 C110 103.3(2) . . ? C111 N104 Ni12 103.37(16) . . ? C120 N104 Ni12 115.04(16) . . ? C110 N104 Ni12 110.67(17) . . ? C11 O10 Ni11 122.22(18) . . ? C11 O10 Ni12 137.88(19) . . ? Ni11 O10 Ni12 97.00(8) . . ? C13 O11 Ni11 118.80(19) . . ? C12S O12S Ni12 120.99(18) . . ? C12S O12S H12S 110(3) . . ? Ni12 O12S H12S 126(3) . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C11 C10 H10D 109.5 . . ? H10A C10 H10D 141.1 . . ? H10B C10 H10D 56.3 . . ? H10C C10 H10D 56.3 . . ? C11 C10 H10E 109.5 . . ? H10A C10 H10E 56.3 . . ? H10B C10 H10E 141.1 . . ? H10C C10 H10E 56.3 . . ? H10D C10 H10E 109.5 . . ? C11 C10 H10F 109.5 . . ? H10A C10 H10F 56.3 . . ? H10B C10 H10F 56.3 . . ? H10C C10 H10F 141.1 . . ? H10D C10 H10F 109.5 . . ? H10E C10 H10F 109.5 . . ? O10 C11 C12 123.9(3) . . ? O10 C11 C10 117.9(3) . . ? C12 C11 C10 118.2(3) . . ? C11 C12 C13 126.2(3) . . ? C11 C12 H12 116.9 . . ? C13 C12 H12 116.9 . . ? O11 C13 C12 125.4(3) . . ? O11 C13 C14 117.3(3) . . ? C12 C13 C14 117.3(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C14 H14D 109.5 . . ? H14A C14 H14D 141.1 . . ? H14B C14 H14D 56.3 . . ? H14C C14 H14D 56.3 . . ? C13 C14 H14E 109.5 . . ? H14A C14 H14E 56.3 . . ? H14B C14 H14E 141.1 . . ? H14C C14 H14E 56.3 . . ? H14D C14 H14E 109.5 . . ? C13 C14 H14F 109.5 . . ? H14A C14 H14F 56.3 . . ? H14B C14 H14F 56.3 . . ? H14C C14 H14F 141.1 . . ? H14D C14 H14F 109.5 . . ? H14E C14 H14F 109.5 . . ? O12S C12S H12A 109.5 . . ? O12S C12S H12B 109.5 . . ? H12A C12S H12B 109.5 . . ? O12S C12S H12C 109.5 . . ? H12A C12S H12C 109.5 . . ? H12B C12S H12C 109.5 . . ? O101 C100 C101 120.2(3) . . ? O101 C100 C105 122.4(3) . . ? C101 C100 C105 117.5(3) . . ? C102 C101 C100 122.0(3) . . ? C102 C101 H101 119.0 . . ? C100 C101 H101 119.0 . . ? C101 C102 C103 120.9(3) . . ? C101 C102 H102 119.6 . . ? C103 C102 H102 119.6 . . ? C104 C103 C102 118.5(3) . . ? C104 C103 H103 120.7 . . ? C102 C103 H103 120.7 . . ? C103 C104 C105 122.4(3) . . ? C103 C104 H104 118.8 . . ? C105 C104 H104 118.8 . . ? C104 C105 C100 118.7(3) . . ? C104 C105 C106 117.7(3) . . ? C100 C105 C106 123.6(3) . . ? N101 C106 C105 126.5(3) . . ? N101 C106 H106 116.7 . . ? C105 C106 H106 116.7 . . ? N101 C107 C108 107.6(2) . . ? N101 C107 H10G 110.2 . . ? C108 C107 H10G 110.2 . . ? N101 C107 H10H 110.2 . . ? C108 C107 H10H 110.2 . . ? H10G C107 H10H 108.5 . . ? N103 C108 C107 112.5(2) . . ? N103 C108 H10I 109.1 . . ? C107 C108 H10I 109.1 . . ? N103 C108 H10J 109.1 . . ? C107 C108 H10J 109.1 . . ? H10I C108 H10J 107.8 . . ? N103 C109 C110 104.4(2) . . ? N103 C109 H10K 110.9 . . ? C110 C109 H10K 110.9 . . ? N103 C109 H10L 110.9 . . ? C110 C109 H10L 110.9 . . ? H10K C109 H10L 108.9 . . ? N104 C110 C109 105.5(2) . . ? N104 C110 H11A 110.6 . . ? C109 C110 H11A 110.6 . . ? N104 C110 H11B 110.6 . . ? C109 C110 H11B 110.6 . . ? H11A C110 H11B 108.8 . . ? N104 C111 C112 111.9(2) . . ? N104 C111 H11C 109.2 . . ? C112 C111 H11C 109.2 . . ? N104 C111 H11D 109.2 . . ? C112 C111 H11D 109.2 . . ? H11C C111 H11D 107.9 . . ? N102 C112 C111 108.9(2) . . ? N102 C112 H11E 109.9 . . ? C111 C112 H11E 109.9 . . ? N102 C112 H11F 109.9 . . ? C111 C112 H11F 109.9 . . ? H11E C112 H11F 108.3 . . ? N102 C113 C114 125.3(3) . . ? N102 C113 H113 117.4 . . ? C114 C113 H113 117.4 . . ? C115 C114 C119 120.0(3) . . ? C115 C114 C113 115.6(3) . . ? C119 C114 C113 124.4(3) . . ? C116 C115 C114 122.1(3) . . ? C116 C115 H115 119.0 . . ? C114 C115 H115 119.0 . . ? C115 C116 C117 118.5(3) . . ? C115 C116 H116 120.8 . . ? C117 C116 H116 120.8 . . ? C118 C117 C116 120.5(3) . . ? C118 C117 H117 119.8 . . ? C116 C117 H117 119.8 . . ? C117 C118 C119 122.6(3) . . ? C117 C118 H118 118.7 . . ? C119 C118 H118 118.7 . . ? O102 C119 C118 119.2(3) . . ? O102 C119 C114 124.6(3) . . ? C118 C119 C114 116.2(3) . . ? N103 C120 N104 101.4(2) . . ? N103 C120 C121 114.3(2) . . ? N104 C120 C121 115.6(2) . . ? N103 C120 H120 108.4 . . ? N104 C120 H120 108.4 . . ? C121 C120 H120 108.4 . . ? C122 C121 C126 120.6(3) . . ? C122 C121 C120 119.8(3) . . ? C126 C121 C120 119.6(3) . . ? C121 C122 C123 121.9(3) . . ? C121 C122 H122 119.1 . . ? C123 C122 H122 119.1 . . ? C122 C123 C124 117.4(3) . . ? C122 C123 H123 121.3 . . ? C124 C123 H123 121.3 . . ? C125 C124 C123 121.4(3) . . ? C125 C124 H124 119.3 . . ? C123 C124 H124 119.3 . . ? C124 C125 C126 121.2(3) . . ? C124 C125 H125 119.4 . . ? C126 C125 H125 119.4 . . ? O103 C126 C125 121.6(3) . . ? O103 C126 C121 121.0(3) . . ? C125 C126 C121 117.4(3) . . ? H1W1 O1W H2W1 106(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N101 Ni11 O101 C100 -33.7(2) . . . . ? O10 Ni11 O101 C100 142.4(2) . . . . ? O11 Ni11 O101 C100 54.1(2) . . . . ? O103 Ni11 O101 C100 -136.7(2) . . . . ? N102 Ni12 O102 C119 -2.3(2) . . . . ? O103 Ni12 O102 C119 96.6(2) . . . . ? O10 Ni12 O102 C119 176.7(2) . . . . ? O12S Ni12 O102 C119 -92.2(2) . . . . ? O102 Ni12 O103 C126 -124.83(19) . . . . ? N102 Ni12 O103 C126 -32.8(2) . . . . ? O10 Ni12 O103 C126 141.58(19) . . . . ? O12S Ni12 O103 C126 127.5(5) . . . . ? N104 Ni12 O103 C126 49.44(19) . . . . ? O102 Ni12 O103 Ni11 111.73(8) . . . . ? N102 Ni12 O103 Ni11 -156.21(9) . . . . ? O10 Ni12 O103 Ni11 18.14(7) . . . . ? O12S Ni12 O103 Ni11 4.1(5) . . . . ? N104 Ni12 O103 Ni11 -73.99(8) . . . . ? O101 Ni11 O103 C126 126.92(18) . . . . ? N101 Ni11 O103 C126 36.81(19) . . . . ? O10 Ni11 O103 C126 -142.08(19) . . . . ? O11 Ni11 O103 C126 -138.1(4) . . . . ? N103 Ni11 O103 C126 -46.33(19) . . . . ? O101 Ni11 O103 Ni12 -109.62(8) . . . . ? N101 Ni11 O103 Ni12 160.28(8) . . . . ? O10 Ni11 O103 Ni12 -18.62(7) . . . . ? O11 Ni11 O103 Ni12 -14.6(4) . . . . ? N103 Ni11 O103 Ni12 77.13(9) . . . . ? O101 Ni11 N101 C106 26.4(2) . . . . ? O10 Ni11 N101 C106 -76.1(13) . . . . ? O11 Ni11 N101 C106 -61.4(2) . . . . ? O103 Ni11 N101 C106 119.6(2) . . . . ? N103 Ni11 N101 C106 -152.5(2) . . . . ? O101 Ni11 N101 C107 -172.0(2) . . . . ? O11 Ni11 N101 C107 100.2(2) . . . . ? O103 Ni11 N101 C107 -78.8(2) . . . . ? N103 Ni11 N101 C107 9.14(19) . . . . ? O102 Ni12 N102 C113 -3.7(3) . . . . ? O103 Ni12 N102 C113 -96.8(3) . . . . ? O10 Ni12 N102 C113 -173.5(8) . . . . ? O12S Ni12 N102 C113 86.3(3) . . . . ? N104 Ni12 N102 C113 176.2(3) . . . . ? O102 Ni12 N102 C112 -179.3(2) . . . . ? O103 Ni12 N102 C112 87.6(2) . . . . ? O12S Ni12 N102 C112 -89.3(2) . . . . ? N104 Ni12 N102 C112 0.6(2) . . . . ? O101 Ni11 N103 C120 -116.3(7) . . . . ? N101 Ni11 N103 C120 -107.31(19) . . . . ? O10 Ni11 N103 C120 76.65(19) . . . . ? O11 Ni11 N103 C120 165.08(18) . . . . ? O103 Ni11 N103 C120 -4.11(18) . . . . ? O101 Ni11 N103 C109 127.8(7) . . . . ? N101 Ni11 N103 C109 136.82(19) . . . . ? O10 Ni11 N103 C109 -39.22(19) . . . . ? O11 Ni11 N103 C109 49.21(19) . . . . ? O103 Ni11 N103 C109 -119.98(19) . . . . ? N101 Ni11 N103 C108 16.21(17) . . . . ? O10 Ni11 N103 C108 -159.83(17) . . . . ? O11 Ni11 N103 C108 -71.40(18) . . . . ? O103 Ni11 N103 C108 119.40(17) . . . . ? N102 Ni12 N104 C111 -23.70(17) . . . . ? O103 Ni12 N104 C111 -122.83(17) . . . . ? O10 Ni12 N104 C111 157.32(17) . . . . ? O12S Ni12 N104 C111 66.15(17) . . . . ? O102 Ni12 N104 C120 100.6(8) . . . . ? N102 Ni12 N104 C120 99.8(2) . . . . ? O103 Ni12 N104 C120 0.70(19) . . . . ? O10 Ni12 N104 C120 -79.15(19) . . . . ? O12S Ni12 N104 C120 -170.32(19) . . . . ? O102 Ni12 N104 C110 -142.8(8) . . . . ? N102 Ni12 N104 C110 -143.62(18) . . . . ? O103 Ni12 N104 C110 117.25(18) . . . . ? O10 Ni12 N104 C110 37.41(18) . . . . ? O12S Ni12 N104 C110 -53.77(18) . . . . ? O101 Ni11 O10 C11 -52.4(2) . . . . ? O11 Ni11 O10 C11 35.3(2) . . . . ? O103 Ni11 O10 C11 -145.5(2) . . . . ? N103 Ni11 O10 C11 125.9(2) . . . . ? O101 Ni11 O10 Ni12 111.43(8) . . . . ? N101 Ni11 O10 Ni12 -146.1(12) . . . . ? O11 Ni11 O10 Ni12 -160.83(8) . . . . ? O103 Ni11 O10 Ni12 18.42(7) . . . . ? N103 Ni11 O10 Ni12 -70.20(9) . . . . ? O102 Ni12 O10 C11 48.7(3) . . . . ? N102 Ni12 O10 C11 -141.5(8) . . . . ? O103 Ni12 O10 C11 140.9(3) . . . . ? O12S Ni12 O10 C11 -41.4(3) . . . . ? N104 Ni12 O10 C11 -131.3(3) . . . . ? O102 Ni12 O10 Ni11 -110.79(8) . . . . ? O103 Ni12 O10 Ni11 -18.63(7) . . . . ? O12S Ni12 O10 Ni11 159.15(8) . . . . ? N104 Ni12 O10 Ni11 69.19(9) . . . . ? O101 Ni11 O11 C13 52.4(2) . . . . ? N101 Ni11 O11 C13 141.8(2) . . . . ? O10 Ni11 O11 C13 -39.2(2) . . . . ? O103 Ni11 O11 C13 -43.2(5) . . . . ? N103 Ni11 O11 C13 -134.8(2) . . . . ? O102 Ni12 O12S C12S 24.9(2) . . . . ? N102 Ni12 O12S C12S -66.7(2) . . . . ? O103 Ni12 O12S C12S 132.8(5) . . . . ? O10 Ni12 O12S C12S 118.9(2) . . . . ? N104 Ni12 O12S C12S -149.3(2) . . . . ? Ni11 O10 C11 C12 -20.8(4) . . . . ? Ni12 O10 C11 C12 -176.5(2) . . . . ? Ni11 O10 C11 C10 159.6(2) . . . . ? Ni12 O10 C11 C10 3.8(4) . . . . ? O10 C11 C12 C13 -4.1(5) . . . . ? C10 C11 C12 C13 175.5(3) . . . . ? Ni11 O11 C13 C12 30.2(4) . . . . ? Ni11 O11 C13 C14 -148.8(2) . . . . ? C11 C12 C13 O11 -2.0(5) . . . . ? C11 C12 C13 C14 177.0(3) . . . . ? Ni11 O101 C100 C101 -152.8(2) . . . . ? Ni11 O101 C100 C105 27.6(4) . . . . ? O101 C100 C101 C102 -177.2(3) . . . . ? C105 C100 C101 C102 2.5(4) . . . . ? C100 C101 C102 C103 -1.2(5) . . . . ? C101 C102 C103 C104 -0.3(5) . . . . ? C102 C103 C104 C105 0.6(5) . . . . ? C103 C104 C105 C100 0.7(5) . . . . ? C103 C104 C105 C106 -178.5(3) . . . . ? O101 C100 C105 C104 177.5(3) . . . . ? C101 C100 C105 C104 -2.2(4) . . . . ? O101 C100 C105 C106 -3.3(4) . . . . ? C101 C100 C105 C106 177.0(3) . . . . ? C107 N101 C106 C105 -174.8(3) . . . . ? Ni11 N101 C106 C105 -14.1(4) . . . . ? C104 C105 C106 N101 175.4(3) . . . . ? C100 C105 C106 N101 -3.8(5) . . . . ? C106 N101 C107 C108 130.5(3) . . . . ? Ni11 N101 C107 C108 -32.0(3) . . . . ? C120 N103 C108 C107 85.1(3) . . . . ? C109 N103 C108 C107 -161.3(2) . . . . ? Ni11 N103 C108 C107 -38.7(3) . . . . ? N101 C107 C108 N103 47.9(3) . . . . ? C120 N103 C109 C110 -35.2(3) . . . . ? C108 N103 C109 C110 -155.7(2) . . . . ? Ni11 N103 C109 C110 87.5(2) . . . . ? C111 N104 C110 C109 142.3(2) . . . . ? C120 N104 C110 C109 20.6(3) . . . . ? Ni12 N104 C110 C109 -103.0(2) . . . . ? N103 C109 C110 N104 8.9(3) . . . . ? C120 N104 C111 C112 -81.7(3) . . . . ? C110 N104 C111 C112 162.3(2) . . . . ? Ni12 N104 C111 C112 43.2(3) . . . . ? C113 N102 C112 C111 -153.2(3) . . . . ? Ni12 N102 C112 C111 22.8(3) . . . . ? N104 C111 C112 N102 -45.3(3) . . . . ? C112 N102 C113 C114 -176.9(3) . . . . ? Ni12 N102 C113 C114 7.6(4) . . . . ? N102 C113 C114 C115 174.1(3) . . . . ? N102 C113 C114 C119 -5.2(5) . . . . ? C119 C114 C115 C116 2.4(5) . . . . ? C113 C114 C115 C116 -177.0(3) . . . . ? C114 C115 C116 C117 -1.2(5) . . . . ? C115 C116 C117 C118 -1.7(5) . . . . ? C116 C117 C118 C119 3.6(5) . . . . ? Ni12 O102 C119 C118 -175.4(2) . . . . ? Ni12 O102 C119 C114 4.8(4) . . . . ? C117 C118 C119 O102 177.8(3) . . . . ? C117 C118 C119 C114 -2.3(4) . . . . ? C115 C114 C119 O102 179.2(3) . . . . ? C113 C114 C119 O102 -1.4(5) . . . . ? C115 C114 C119 C118 -0.6(4) . . . . ? C113 C114 C119 C118 178.8(3) . . . . ? C109 N103 C120 N104 48.4(2) . . . . ? C108 N103 C120 N104 167.3(2) . . . . ? Ni11 N103 C120 N104 -74.3(2) . . . . ? C109 N103 C120 C121 173.5(2) . . . . ? C108 N103 C120 C121 -67.6(3) . . . . ? Ni11 N103 C120 C121 50.8(3) . . . . ? C111 N104 C120 N103 -163.6(2) . . . . ? C110 N104 C120 N103 -42.7(2) . . . . ? Ni12 N104 C120 N103 78.0(2) . . . . ? C111 N104 C120 C121 72.1(3) . . . . ? C110 N104 C120 C121 -166.9(2) . . . . ? Ni12 N104 C120 C121 -46.2(3) . . . . ? N103 C120 C121 C122 118.3(3) . . . . ? N104 C120 C121 C122 -124.4(3) . . . . ? N103 C120 C121 C126 -61.5(3) . . . . ? N104 C120 C121 C126 55.7(4) . . . . ? C126 C121 C122 C123 0.5(5) . . . . ? C120 C121 C122 C123 -179.4(3) . . . . ? C121 C122 C123 C124 -1.8(5) . . . . ? C122 C123 C124 C125 0.6(5) . . . . ? C123 C124 C125 C126 1.9(5) . . . . ? Ni12 O103 C126 C125 121.9(2) . . . . ? Ni11 O103 C126 C125 -125.8(2) . . . . ? Ni12 O103 C126 C121 -58.5(3) . . . . ? Ni11 O103 C126 C121 53.8(3) . . . . ? C124 C125 C126 O103 176.5(3) . . . . ? C124 C125 C126 C121 -3.2(4) . . . . ? C122 C121 C126 O103 -177.6(3) . . . . ? C120 C121 C126 O103 2.2(4) . . . . ? C122 C121 C126 C125 2.0(4) . . . . ? C120 C121 C126 C125 -178.2(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O12S H12S O1W 0.77(3) 1.88(3) 2.634(3) 168(4) 4_565 O1W H1W1 O101 0.82(4) 1.84(4) 2.658(3) 175(3) . O1W H2W1 O102 0.73(4) 2.07(4) 2.793(3) 169(4) . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.501 _refine_diff_density_min -0.391 _refine_diff_density_rms 0.092 #END data_2.1.5H2O _database_code_depnum_ccdc_archive 'CCDC 606601' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H35 Br3 N4 Ni2 O6, 1.5(H2 O)' _chemical_formula_sum 'C33 H38 Br3 N4 Ni2 O7.50' _chemical_formula_weight 967.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 20.515(5) _cell_length_b 14.726(5) _cell_length_c 24.311(5) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_volume 7344(3) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7073 _cell_measurement_theta_min 0.98 _cell_measurement_theta_max 66.6 _exptl_crystal_description Plate _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.751 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3880 _exptl_absorpt_coefficient_mu 4.342 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.5099 _exptl_absorpt_correction_T_max 0.8808 _exptl_absorpt_process_details SADABS-2004/1 _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'FR591-KappaCCD2000 Bruker-Nonius' _diffrn_measurement_method 'omega/phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 131465 _diffrn_reflns_av_R_equivalents 0.0848 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.05 _reflns_number_total 6491 _reflns_number_gt 5983 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect - HKL2000' _computing_cell_refinement 'Nonius Collect - HKL2000' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR-92 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'Wingx (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1314P)^2^+31.8647P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6491 _refine_ls_number_parameters 491 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0809 _refine_ls_R_factor_gt 0.0767 _refine_ls_wR_factor_ref 0.2173 _refine_ls_wR_factor_gt 0.2122 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni11 Ni 0.12253(5) 0.31106(7) 0.09225(4) 0.0469(3) Uani 1 1 d . A . Ni12 Ni 0.26049(5) 0.37001(6) 0.12916(4) 0.0419(3) Uani 1 1 d . A . O101 O 0.10871(19) 0.1880(3) 0.12644(16) 0.0290(8) Uani 1 1 d . . . O102 O 0.29934(19) 0.2656(3) 0.17143(16) 0.0297(8) Uani 1 1 d . . . O103 O 0.2194(2) 0.2850(3) 0.07035(16) 0.0303(9) Uani 1 1 d . . . N101 N 0.0737(3) 0.2701(4) 0.0245(2) 0.0410(13) Uani 1 1 d . . . N102 N 0.3467(3) 0.3935(3) 0.09217(19) 0.0295(10) Uani 1 1 d . . . N103 N 0.1279(3) 0.4397(4) 0.0495(2) 0.0359(12) Uani 1 1 d . . . N104 N 0.2290(2) 0.4849(3) 0.07791(18) 0.0261(10) Uani 1 1 d . . . O10 O 0.1668(2) 0.3547(3) 0.16219(15) 0.0278(8) Uani 1 1 d . . . O11 O 0.0347(2) 0.3502(3) 0.12444(19) 0.0418(11) Uani 1 1 d . . . O12S O 0.2854(2) 0.4623(3) 0.19315(16) 0.0316(9) Uani 1 1 d . . . H12S H 0.2813 0.5085 0.1933 0.080 Uiso 1 1 d . . . C12S C 0.3342(3) 0.4406(4) 0.2328(3) 0.0371(14) Uani 1 1 d . A . H12A H 0.3388 0.4911 0.2588 0.056 Uiso 1 1 calc R . . H12B H 0.3759 0.4302 0.2142 0.056 Uiso 1 1 calc R . . H12C H 0.3215 0.3856 0.2528 0.056 Uiso 1 1 calc R . . C11 C 0.1394(3) 0.3508(4) 0.2098(2) 0.0330(13) Uani 1 1 d . A . C10 C 0.1822(4) 0.3524(5) 0.2595(2) 0.0410(15) Uani 1 1 d . . . H10A H 0.2279 0.3561 0.2481 0.062 Uiso 0.19(9) 1 calc PR A . H10B H 0.1754 0.2968 0.2809 0.062 Uiso 0.19(9) 1 calc PR . . H10C H 0.1713 0.4054 0.2821 0.062 Uiso 0.19(9) 1 calc PR . . H10D H 0.1552 0.3494 0.2927 0.062 Uiso 0.81(9) 1 calc PR . . H10E H 0.2077 0.4087 0.2598 0.062 Uiso 0.81(9) 1 calc PR . . H10F H 0.2118 0.3002 0.2586 0.062 Uiso 0.81(9) 1 calc PR . . C12 C 0.0718(3) 0.3451(5) 0.2167(3) 0.0417(15) Uani 1 1 d . . . H12 H 0.0567 0.3404 0.2535 0.050 Uiso 1 1 calc R A . C13 C 0.0232(4) 0.3454(5) 0.1753(3) 0.0462(17) Uani 1 1 d . A . C14 C -0.0468(4) 0.3402(7) 0.1917(4) 0.063(2) Uani 1 1 d . . . H14A H -0.0742 0.3407 0.1588 0.095 Uiso 0.12(11) 1 calc PR A . H14B H -0.0577 0.3925 0.2149 0.095 Uiso 0.12(11) 1 calc PR . . H14C H -0.0543 0.2840 0.2124 0.095 Uiso 0.12(11) 1 calc PR . . H14D H -0.0499 0.3374 0.2319 0.095 Uiso 0.88(11) 1 calc PR . . H14E H -0.0665 0.2856 0.1758 0.095 Uiso 0.88(11) 1 calc PR . . H14F H -0.0698 0.3941 0.1783 0.095 Uiso 0.88(11) 1 calc PR . . C100 C 0.0586(3) 0.1378(4) 0.1175(2) 0.0288(12) Uani 1 1 d . A . C101 C 0.0383(3) 0.0742(4) 0.1580(2) 0.0321(12) Uani 1 1 d . . . H101 H 0.0605 0.0729 0.1923 0.038 Uiso 1 1 calc R . . C102 C -0.0123(3) 0.0146(4) 0.1496(2) 0.0329(12) Uani 1 1 d . . . H102 H -0.0240 -0.0273 0.1776 0.039 Uiso 1 1 calc R . . C103 C -0.0467(3) 0.0153(4) 0.0998(3) 0.0380(14) Uani 1 1 d . . . Br11 Br -0.11384(4) -0.07060(5) 0.08697(3) 0.0459(2) Uani 1 1 d . . . C104 C -0.0297(3) 0.0781(4) 0.0596(3) 0.0366(14) Uani 1 1 d . A . H104 H -0.0532 0.0790 0.0260 0.044 Uiso 1 1 calc R . . C105 C 0.0214(3) 0.1405(4) 0.0675(2) 0.0331(13) Uani 1 1 d . . . C106 C 0.0319(3) 0.2050(5) 0.0242(3) 0.0421(15) Uani 1 1 d . A . H106 H 0.0054 0.1992 -0.0076 0.050 Uiso 1 1 calc R . . C107 C 0.0795(11) 0.3307(13) -0.0222(6) 0.031(4) Uani 0.66(6) 1 d P A 1 H10G H 0.0416 0.3240 -0.0470 0.037 Uiso 0.66(6) 1 calc PR A 1 H10H H 0.1198 0.3175 -0.0432 0.037 Uiso 0.66(6) 1 calc PR A 1 C108 C 0.0819(11) 0.4245(13) 0.0014(9) 0.038(4) Uani 0.66(6) 1 d P A 1 H10J H 0.0374 0.4411 0.0134 0.045 Uiso 0.66(6) 1 calc PR A 1 H10K H 0.0943 0.4669 -0.0284 0.045 Uiso 0.66(6) 1 calc PR A 1 C17' C 0.0624(16) 0.350(2) -0.0118(14) 0.030(7) Uiso 0.34(6) 1 d P A 2 H17A H 0.0939 0.3474 -0.0426 0.036 Uiso 0.34(6) 1 calc PR A 2 H17B H 0.0182 0.3450 -0.0278 0.036 Uiso 0.34(6) 1 calc PR A 2 C18' C 0.0678(15) 0.439(2) 0.0132(13) 0.029(7) Uiso 0.34(6) 1 d P A 2 H18A H 0.0286 0.4525 0.0355 0.035 Uiso 0.34(6) 1 calc PR A 2 H18B H 0.0717 0.4866 -0.0156 0.035 Uiso 0.34(6) 1 calc PR A 2 C109 C 0.1154(3) 0.5197(4) 0.0854(3) 0.0435(16) Uani 1 1 d . A . H10L H 0.0850 0.5039 0.1156 0.052 Uiso 1 1 calc R . . H10M H 0.0968 0.5706 0.0640 0.052 Uiso 1 1 calc R . . C110 C 0.1822(3) 0.5442(4) 0.1080(3) 0.0331(13) Uani 1 1 d . A . H11A H 0.1920 0.6091 0.1012 0.040 Uiso 1 1 calc R . . H11B H 0.1843 0.5326 0.1480 0.040 Uiso 1 1 calc R . . C111 C 0.2916(3) 0.5324(4) 0.0660(2) 0.0277(11) Uani 1 1 d . A . H11C H 0.3045 0.5684 0.0986 0.033 Uiso 1 1 calc R . . H11D H 0.2850 0.5750 0.0350 0.033 Uiso 1 1 calc R . . C112 C 0.3454(3) 0.4676(4) 0.0518(2) 0.0296(12) Uani 1 1 d . A . H11E H 0.3382 0.4425 0.0145 0.036 Uiso 1 1 calc R . . H11F H 0.3877 0.4999 0.0519 0.036 Uiso 1 1 calc R . . C113 C 0.4016(3) 0.3555(4) 0.1034(2) 0.0306(12) Uani 1 1 d . . . H113 H 0.4392 0.3785 0.0854 0.037 Uiso 1 1 calc R . . C114 C 0.4110(3) 0.2811(4) 0.1410(2) 0.0294(12) Uani 1 1 d . . . C115 C 0.4754(3) 0.2484(4) 0.1449(2) 0.0337(12) Uani 1 1 d . . . H115 H 0.5090 0.2768 0.1243 0.040 Uiso 1 1 calc R . . C116 C 0.4901(3) 0.1758(4) 0.1782(2) 0.0389(14) Uani 1 1 d . . . Br12 Br 0.57802(4) 0.13345(6) 0.18165(3) 0.0529(3) Uani 1 1 d . . . C117 C 0.4414(3) 0.1344(4) 0.2093(2) 0.0367(14) Uani 1 1 d . . . H117 H 0.4517 0.0844 0.2324 0.044 Uiso 1 1 calc R . . C118 C 0.3787(3) 0.1660(4) 0.2066(2) 0.0322(13) Uani 1 1 d . . . H118 H 0.3463 0.1373 0.2284 0.039 Uiso 1 1 calc R A . C119 C 0.3604(3) 0.2395(4) 0.1726(2) 0.0283(11) Uani 1 1 d . . . C120 C 0.1936(3) 0.4604(4) 0.0271(2) 0.0311(12) Uani 1 1 d . A . H120 H 0.1902 0.5157 0.0035 0.037 Uiso 1 1 calc R . . C121 C 0.2227(4) 0.3866(4) -0.0059(2) 0.0382(15) Uani 1 1 d . . . C122 C 0.2460(8) 0.3971(9) -0.0605(4) 0.035(3) Uani 0.641(9) 1 d P A 3 H122 H 0.2400 0.4542 -0.0780 0.042 Uiso 0.641(9) 1 calc PR A 3 C123 C 0.2763(8) 0.3302(8) -0.0892(5) 0.051(4) Uani 0.641(9) 1 d P A 3 Br13 Br 0.2991(4) 0.34715(17) -0.16406(11) 0.104(2) Uani 0.641(9) 1 d P A 3 C124 C 0.2931(8) 0.2511(7) -0.0638(5) 0.059(4) Uani 0.641(9) 1 d P A 3 H124 H 0.3171 0.2064 -0.0835 0.071 Uiso 0.641(9) 1 calc PR A 3 C125 C 0.2756(6) 0.2349(6) -0.0097(4) 0.039(3) Uani 0.641(9) 1 d P A 3 H125 H 0.2862 0.1784 0.0068 0.047 Uiso 0.641(9) 1 calc PR A 3 C126 C 0.2427(7) 0.3003(8) 0.0210(5) 0.025(2) Uani 0.641(9) 1 d P A 3 C22' C 0.2230(10) 0.4131(16) -0.0622(10) 0.026(6) Uiso 0.359(9) 1 d P A 4 H22' H 0.2112 0.4721 -0.0744 0.031 Uiso 0.359(9) 1 calc PR A 4 C23' C 0.2416(13) 0.3468(18) -0.0964(11) 0.051(7) Uiso 0.359(9) 1 d P A 4 Br3' Br 0.2525(3) 0.3714(3) -0.17360(10) 0.0615(14) Uani 0.359(9) 1 d P A 4 C24' C 0.2482(14) 0.2631(19) -0.0778(11) 0.060(6) Uiso 0.359(9) 1 d P A 4 H24' H 0.2609 0.2160 -0.1023 0.072 Uiso 0.359(9) 1 calc PR A 4 C25' C 0.2368(12) 0.2430(17) -0.0227(9) 0.049(5) Uiso 0.359(9) 1 d P A 4 H25' H 0.2392 0.1813 -0.0117 0.059 Uiso 0.359(9) 1 calc PR A 4 C26' C 0.2231(10) 0.3032(18) 0.0145(10) 0.023(6) Uiso 0.359(9) 1 d P A 4 O1W O 0.2055(2) 0.1391(3) 0.19551(16) 0.0314(9) Uani 1 1 d . . . H1W1 H 0.2271 0.1790 0.1936 0.080 Uiso 1 1 d . . . H1W2 H 0.1733 0.1598 0.1770 0.080 Uiso 1 1 d . . . O2W O -0.0722(7) 0.3589(11) 0.0482(7) 0.085(4) Uiso 0.50 1 d P . . H2W1 H -0.1059 0.3265 0.0518 0.080 Uiso 0.50 1 d P . . H2W2 H -0.0396 0.3559 0.0707 0.080 Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni11 0.0558(6) 0.0427(6) 0.0423(5) 0.0032(4) -0.0033(4) -0.0015(4) Ni12 0.0544(6) 0.0329(5) 0.0385(5) 0.0006(3) 0.0008(4) 0.0001(4) O101 0.036(2) 0.025(2) 0.0260(19) 0.0016(16) -0.0030(16) -0.0037(16) O102 0.037(2) 0.0212(19) 0.031(2) 0.0031(16) -0.0003(17) 0.0009(16) O103 0.046(2) 0.0211(19) 0.0241(19) -0.0019(15) 0.0070(17) -0.0065(17) N101 0.049(3) 0.041(3) 0.033(3) 0.012(2) -0.007(2) -0.014(3) N102 0.045(3) 0.019(2) 0.025(2) 0.0003(18) 0.001(2) -0.001(2) N103 0.039(3) 0.032(3) 0.037(3) 0.008(2) -0.007(2) -0.005(2) N104 0.040(3) 0.014(2) 0.025(2) 0.0013(17) 0.0002(19) 0.0018(19) O10 0.040(2) 0.0216(19) 0.0219(19) -0.0008(15) 0.0023(16) 0.0008(16) O11 0.045(3) 0.038(2) 0.043(3) 0.009(2) 0.003(2) 0.002(2) O12S 0.053(3) 0.016(2) 0.026(2) 0.0001(16) -0.0064(18) -0.0026(19) C12S 0.052(4) 0.027(3) 0.033(3) 0.002(2) -0.015(3) -0.008(3) C11 0.050(4) 0.024(3) 0.026(3) -0.006(2) 0.009(3) -0.002(3) C10 0.060(4) 0.040(4) 0.023(3) -0.001(2) 0.001(3) -0.008(3) C12 0.050(4) 0.040(4) 0.035(3) -0.002(3) 0.014(3) 0.004(3) C13 0.046(4) 0.035(3) 0.057(4) 0.002(3) 0.013(3) 0.009(3) C14 0.048(4) 0.071(6) 0.070(5) 0.014(4) 0.023(4) 0.008(4) C100 0.040(3) 0.023(3) 0.023(3) -0.001(2) 0.000(2) 0.003(2) C101 0.045(3) 0.024(3) 0.028(3) 0.000(2) 0.000(2) -0.002(2) C102 0.042(3) 0.026(3) 0.031(3) 0.004(2) 0.000(2) -0.001(2) C103 0.050(4) 0.030(3) 0.034(3) 0.005(3) 0.002(3) 0.003(3) Br11 0.0531(4) 0.0372(4) 0.0474(4) 0.0097(3) -0.0098(3) -0.0128(3) C104 0.047(3) 0.034(3) 0.030(3) 0.005(2) -0.008(3) -0.006(3) C105 0.038(3) 0.033(3) 0.028(3) 0.002(2) -0.004(2) -0.008(3) C106 0.051(4) 0.043(4) 0.032(3) 0.005(3) -0.016(3) -0.015(3) C107 0.044(7) 0.033(7) 0.015(5) 0.002(4) -0.002(5) -0.003(6) C108 0.042(8) 0.038(7) 0.033(7) 0.012(6) -0.007(6) 0.006(6) C109 0.050(4) 0.021(3) 0.059(4) 0.010(3) -0.003(3) 0.006(3) C110 0.044(3) 0.019(3) 0.037(3) -0.001(2) 0.006(3) 0.011(2) C111 0.038(3) 0.018(3) 0.027(3) 0.005(2) -0.001(2) -0.003(2) C112 0.039(3) 0.020(3) 0.030(3) 0.007(2) 0.005(2) 0.000(2) C113 0.038(3) 0.024(3) 0.030(3) -0.001(2) 0.006(2) 0.001(2) C114 0.035(3) 0.024(3) 0.030(3) -0.002(2) 0.001(2) 0.006(2) C115 0.040(3) 0.033(3) 0.028(3) -0.001(2) 0.004(2) 0.001(3) C116 0.055(4) 0.032(3) 0.029(3) -0.003(2) -0.004(3) 0.005(3) Br12 0.0503(4) 0.0606(5) 0.0479(4) 0.0129(3) 0.0017(3) 0.0184(3) C117 0.053(4) 0.032(3) 0.025(3) 0.005(2) -0.002(3) 0.009(3) C118 0.043(3) 0.024(3) 0.029(3) 0.002(2) -0.002(2) 0.003(2) C119 0.039(3) 0.019(3) 0.027(3) -0.004(2) -0.004(2) 0.001(2) C120 0.042(3) 0.028(3) 0.024(3) 0.012(2) -0.006(2) -0.006(2) C121 0.063(4) 0.031(3) 0.021(3) 0.001(2) 0.002(3) -0.021(3) C122 0.050(8) 0.031(6) 0.023(5) 0.002(4) 0.005(5) -0.012(6) C123 0.083(10) 0.030(6) 0.039(6) -0.008(5) 0.025(6) -0.027(7) Br13 0.213(5) 0.0594(11) 0.0383(10) -0.0101(8) 0.057(2) -0.0333(19) C124 0.114(12) 0.020(5) 0.042(6) -0.007(4) 0.043(7) -0.002(6) C125 0.061(7) 0.013(4) 0.042(6) -0.003(4) 0.033(5) -0.003(4) C126 0.028(6) 0.024(5) 0.022(5) -0.002(4) 0.004(5) -0.012(5) Br3' 0.104(3) 0.0552(18) 0.0253(11) 0.0017(9) 0.0119(13) -0.0185(18) O1W 0.047(2) 0.0196(19) 0.028(2) 0.0029(15) -0.0026(18) 0.0002(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni11 O101 2.014(4) . ? Ni11 N101 2.019(5) . ? Ni11 O10 2.032(4) . ? Ni11 O11 2.047(5) . ? Ni11 O103 2.093(4) . ? Ni11 N103 2.164(5) . ? Ni12 O102 2.014(4) . ? Ni12 N102 2.014(5) . ? Ni12 O103 2.079(4) . ? Ni12 O10 2.095(4) . ? Ni12 O12S 2.128(4) . ? Ni12 N104 2.198(4) . ? O101 C100 1.286(7) . ? O102 C119 1.310(7) . ? O103 C126 1.310(11) . ? O103 C26' 1.39(3) . ? N101 C106 1.287(8) . ? N101 C107 1.449(11) . ? N101 C17' 1.50(3) . ? N102 C113 1.287(8) . ? N102 C112 1.468(7) . ? N103 C120 1.484(8) . ? N103 C109 1.489(9) . ? N103 C18' 1.51(3) . ? N103 C108 1.519(14) . ? N104 C120 1.477(7) . ? N104 C111 1.490(7) . ? N104 C110 1.490(7) . ? O10 C11 1.287(7) . ? O11 C13 1.260(9) . ? O12S C12S 1.427(7) . ? O12S H12S 0.69 . ? C12S H12A 0.9800 . ? C12S H12B 0.9800 . ? C12S H12C 0.9800 . ? C11 C12 1.400(10) . ? C11 C10 1.494(9) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C10 H10D 0.9800 . ? C10 H10E 0.9800 . ? C10 H10F 0.9800 . ? C12 C13 1.418(11) . ? C12 H12 0.9500 . ? C13 C14 1.492(10) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C14 H14D 0.9800 . ? C14 H14E 0.9800 . ? C14 H14F 0.9800 . ? C100 C101 1.422(8) . ? C100 C105 1.435(8) . ? C101 C102 1.375(9) . ? C101 H101 0.9500 . ? C102 C103 1.399(9) . ? C102 H102 0.9500 . ? C103 C104 1.391(9) . ? C103 Br11 1.897(7) . ? C104 C105 1.407(9) . ? C104 H104 0.9500 . ? C105 C106 1.434(9) . ? C106 H106 0.9500 . ? C107 C108 1.496(19) . ? C107 H10G 0.9900 . ? C107 H10H 0.9900 . ? C108 H10J 0.9900 . ? C108 H10K 0.9900 . ? C17' C18' 1.45(4) . ? C17' H17A 0.9900 . ? C17' H17B 0.9900 . ? C18' H18A 0.9900 . ? C18' H18B 0.9900 . ? C109 C110 1.518(9) . ? C109 H10L 0.9900 . ? C109 H10M 0.9900 . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 C112 1.501(8) . ? C111 H11C 0.9900 . ? C111 H11D 0.9900 . ? C112 H11E 0.9900 . ? C112 H11F 0.9900 . ? C113 C114 1.438(8) . ? C113 H113 0.9500 . ? C114 C115 1.409(8) . ? C114 C119 1.431(8) . ? C115 C116 1.374(9) . ? C115 H115 0.9500 . ? C116 C117 1.393(10) . ? C116 Br12 1.911(7) . ? C117 C118 1.368(9) . ? C117 H117 0.9500 . ? C118 C119 1.414(8) . ? C118 H118 0.9500 . ? C120 C121 1.476(9) . ? C120 H120 1.0000 . ? C121 C26' 1.32(3) . ? C121 C122 1.420(12) . ? C121 C22' 1.42(2) . ? C121 C126 1.487(15) . ? C122 C123 1.358(19) . ? C122 H122 0.9500 . ? C123 C124 1.362(19) . ? C123 Br13 1.895(11) . ? C124 C125 1.385(14) . ? C124 H124 0.9500 . ? C125 C126 1.393(15) . ? C125 H125 0.9500 . ? C22' C23' 1.34(4) . ? C22' H22' 0.9500 . ? C23' C24' 1.32(4) . ? C23' Br3' 1.92(3) . ? C24' C25' 1.39(3) . ? C24' H24' 0.9500 . ? C25' C26' 1.30(3) . ? C25' H25' 0.9500 . ? O1W H1W1 0.7374 . ? O1W H1W2 0.8554 . ? O2W H2W1 0.8439 . ? O2W H2W2 0.8659 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O101 Ni11 N101 89.89(19) . . ? O101 Ni11 O10 90.14(16) . . ? N101 Ni11 O10 176.8(2) . . ? O101 Ni11 O11 88.37(17) . . ? N101 Ni11 O11 87.7(2) . . ? O10 Ni11 O11 89.10(18) . . ? O101 Ni11 O103 94.22(16) . . ? N101 Ni11 O103 102.1(2) . . ? O10 Ni11 O103 81.17(16) . . ? O11 Ni11 O103 169.93(18) . . ? O101 Ni11 N103 173.40(18) . . ? N101 Ni11 N103 84.0(2) . . ? O10 Ni11 N103 95.87(18) . . ? O11 Ni11 N103 89.0(2) . . ? O103 Ni11 N103 89.42(18) . . ? O102 Ni12 N102 90.66(18) . . ? O102 Ni12 O103 92.96(16) . . ? N102 Ni12 O103 98.77(18) . . ? O102 Ni12 O10 94.91(16) . . ? N102 Ni12 O10 174.35(18) . . ? O103 Ni12 O10 80.04(15) . . ? O102 Ni12 O12S 91.12(17) . . ? N102 Ni12 O12S 90.32(18) . . ? O103 Ni12 O12S 169.99(18) . . ? O10 Ni12 O12S 90.50(17) . . ? O102 Ni12 N104 173.31(17) . . ? N102 Ni12 N104 82.68(19) . . ? O103 Ni12 N104 87.40(17) . . ? O10 Ni12 N104 91.73(17) . . ? O12S Ni12 N104 89.62(17) . . ? C100 O101 Ni11 124.1(4) . . ? C119 O102 Ni12 127.8(4) . . ? C126 O103 Ni12 112.2(6) . . ? C26' O103 Ni12 122.4(11) . . ? C126 O103 Ni11 123.2(8) . . ? C26' O103 Ni11 105.3(9) . . ? Ni12 O103 Ni11 95.71(16) . . ? C106 N101 C107 120.6(6) . . ? C106 N101 C17' 118.9(11) . . ? C106 N101 Ni11 123.9(4) . . ? C107 N101 Ni11 114.5(5) . . ? C17' N101 Ni11 108.8(12) . . ? C113 N102 C112 118.8(5) . . ? C113 N102 Ni12 126.7(4) . . ? C112 N102 Ni12 114.2(4) . . ? C120 N103 C109 102.0(5) . . ? C120 N103 C18' 121.8(14) . . ? C109 N103 C18' 101.8(14) . . ? C120 N103 C108 108.2(11) . . ? C109 N103 C108 117.5(12) . . ? C120 N103 Ni11 113.7(4) . . ? C109 N103 Ni11 113.7(4) . . ? C18' N103 Ni11 103.6(12) . . ? C108 N103 Ni11 102.1(6) . . ? C120 N104 C111 112.1(4) . . ? C120 N104 C110 103.6(4) . . ? C111 N104 C110 112.0(4) . . ? C120 N104 Ni12 115.5(3) . . ? C111 N104 Ni12 102.6(3) . . ? C110 N104 Ni12 111.3(3) . . ? C11 O10 Ni11 122.9(4) . . ? C11 O10 Ni12 138.5(4) . . ? Ni11 O10 Ni12 97.08(16) . . ? C13 O11 Ni11 121.6(5) . . ? C12S O12S Ni12 121.3(4) . . ? C12S O12S H12S 108 . . ? Ni12 O12S H12S 127 . . ? O12S C12S H12A 109.5 . . ? O12S C12S H12B 109.5 . . ? H12A C12S H12B 109.5 . . ? O12S C12S H12C 109.5 . . ? H12A C12S H12C 109.5 . . ? H12B C12S H12C 109.5 . . ? O10 C11 C12 122.9(6) . . ? O10 C11 C10 118.1(6) . . ? C12 C11 C10 119.0(6) . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C11 C10 H10D 109.5 . . ? H10A C10 H10D 141.1 . . ? H10B C10 H10D 56.3 . . ? H10C C10 H10D 56.3 . . ? C11 C10 H10E 109.5 . . ? H10A C10 H10E 56.3 . . ? H10B C10 H10E 141.1 . . ? H10C C10 H10E 56.3 . . ? H10D C10 H10E 109.5 . . ? C11 C10 H10F 109.5 . . ? H10A C10 H10F 56.3 . . ? H10B C10 H10F 56.3 . . ? H10C C10 H10F 141.1 . . ? H10D C10 H10F 109.5 . . ? H10E C10 H10F 109.5 . . ? C11 C12 C13 127.7(6) . . ? C11 C12 H12 116.2 . . ? C13 C12 H12 116.2 . . ? O11 C13 C12 124.4(6) . . ? O11 C13 C14 116.5(7) . . ? C12 C13 C14 119.1(7) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C14 H14D 109.5 . . ? H14A C14 H14D 141.1 . . ? H14B C14 H14D 56.3 . . ? H14C C14 H14D 56.3 . . ? C13 C14 H14E 109.5 . . ? H14A C14 H14E 56.3 . . ? H14B C14 H14E 141.1 . . ? H14C C14 H14E 56.3 . . ? H14D C14 H14E 109.5 . . ? C13 C14 H14F 109.5 . . ? H14A C14 H14F 56.3 . . ? H14B C14 H14F 56.3 . . ? H14C C14 H14F 141.1 . . ? H14D C14 H14F 109.5 . . ? H14E C14 H14F 109.5 . . ? O101 C100 C101 119.7(5) . . ? O101 C100 C105 123.6(5) . . ? C101 C100 C105 116.7(5) . . ? C102 C101 C100 122.5(6) . . ? C102 C101 H101 118.7 . . ? C100 C101 H101 118.7 . . ? C101 C102 C103 120.3(6) . . ? C101 C102 H102 119.8 . . ? C103 C102 H102 119.8 . . ? C104 C103 C102 119.1(6) . . ? C104 C103 Br11 120.6(5) . . ? C102 C103 Br11 120.2(5) . . ? C103 C104 C105 121.7(6) . . ? C103 C104 H104 119.2 . . ? C105 C104 H104 119.2 . . ? C104 C105 C106 116.4(5) . . ? C104 C105 C100 119.6(5) . . ? C106 C105 C100 124.0(5) . . ? N101 C106 C105 126.1(6) . . ? N101 C106 H106 116.9 . . ? C105 C106 H106 116.9 . . ? N101 C107 C108 105.7(10) . . ? N101 C107 H10G 110.6 . . ? C108 C107 H10G 110.6 . . ? N101 C107 H10H 110.6 . . ? C108 C107 H10H 110.6 . . ? H10G C107 H10H 108.7 . . ? C107 C108 N103 116.8(10) . . ? C107 C108 H10J 108.1 . . ? N103 C108 H10J 108.1 . . ? C107 C108 H10K 108.1 . . ? N103 C108 H10K 108.1 . . ? H10J C108 H10K 107.3 . . ? C18' C17' N101 117(2) . . ? C18' C17' H17A 108.0 . . ? N101 C17' H17A 108.0 . . ? C18' C17' H17B 108.0 . . ? N101 C17' H17B 108.0 . . ? H17A C17' H17B 107.3 . . ? C17' C18' N103 108(2) . . ? C17' C18' H18A 110.1 . . ? N103 C18' H18A 110.1 . . ? C17' C18' H18B 110.1 . . ? N103 C18' H18B 110.1 . . ? H18A C18' H18B 108.4 . . ? N103 C109 C110 104.2(5) . . ? N103 C109 H10L 110.9 . . ? C110 C109 H10L 110.9 . . ? N103 C109 H10M 110.9 . . ? C110 C109 H10M 110.9 . . ? H10L C109 H10M 108.9 . . ? N104 C110 C109 105.4(5) . . ? N104 C110 H11A 110.7 . . ? C109 C110 H11A 110.7 . . ? N104 C110 H11B 110.7 . . ? C109 C110 H11B 110.7 . . ? H11A C110 H11B 108.8 . . ? N104 C111 C112 112.3(4) . . ? N104 C111 H11C 109.1 . . ? C112 C111 H11C 109.1 . . ? N104 C111 H11D 109.1 . . ? C112 C111 H11D 109.1 . . ? H11C C111 H11D 107.9 . . ? N102 C112 C111 109.4(4) . . ? N102 C112 H11E 109.8 . . ? C111 C112 H11E 109.8 . . ? N102 C112 H11F 109.8 . . ? C111 C112 H11F 109.8 . . ? H11E C112 H11F 108.2 . . ? N102 C113 C114 125.8(6) . . ? N102 C113 H113 117.1 . . ? C114 C113 H113 117.1 . . ? C115 C114 C119 119.9(5) . . ? C115 C114 C113 115.5(5) . . ? C119 C114 C113 124.7(5) . . ? C116 C115 C114 120.8(6) . . ? C116 C115 H115 119.6 . . ? C114 C115 H115 119.6 . . ? C115 C116 C117 120.2(6) . . ? C115 C116 Br12 119.1(5) . . ? C117 C116 Br12 120.7(5) . . ? C118 C117 C116 119.9(6) . . ? C118 C117 H117 120.1 . . ? C116 C117 H117 120.1 . . ? C117 C118 C119 122.7(6) . . ? C117 C118 H118 118.7 . . ? C119 C118 H118 118.7 . . ? O102 C119 C118 119.5(5) . . ? O102 C119 C114 123.9(5) . . ? C118 C119 C114 116.6(5) . . ? C121 C120 N104 115.8(5) . . ? C121 C120 N103 114.5(5) . . ? N104 C120 N103 101.0(4) . . ? C121 C120 H120 108.4 . . ? N104 C120 H120 108.4 . . ? N103 C120 H120 108.4 . . ? C26' C121 C122 116.6(13) . . ? C26' C121 C22' 127.8(15) . . ? C26' C121 C120 118.8(12) . . ? C122 C121 C120 124.4(8) . . ? C22' C121 C120 108.9(10) . . ? C122 C121 C126 114.3(9) . . ? C22' C121 C126 131.0(11) . . ? C120 C121 C126 120.1(6) . . ? C123 C122 C121 123.8(11) . . ? C123 C122 H122 118.1 . . ? C121 C122 H122 118.1 . . ? C122 C123 C124 120.3(10) . . ? C122 C123 Br13 120.7(10) . . ? C124 C123 Br13 119.0(9) . . ? C123 C124 C125 120.7(10) . . ? C123 C124 H124 119.6 . . ? C125 C124 H124 119.6 . . ? C124 C125 C126 121.1(10) . . ? C124 C125 H125 119.4 . . ? C126 C125 H125 119.4 . . ? O103 C126 C125 123.3(11) . . ? O103 C126 C121 116.7(10) . . ? C125 C126 C121 119.2(9) . . ? C23' C22' C121 114(2) . . ? C23' C22' H22' 123.2 . . ? C121 C22' H22' 123.2 . . ? C24' C23' C22' 120(3) . . ? C24' C23' Br3' 120(2) . . ? C22' C23' Br3' 120(2) . . ? C23' C24' C25' 121(3) . . ? C23' C24' H24' 119.6 . . ? C25' C24' H24' 119.6 . . ? C26' C25' C24' 124(2) . . ? C26' C25' H25' 117.9 . . ? C24' C25' H25' 117.9 . . ? C25' C26' C121 112(2) . . ? C25' C26' O103 124(2) . . ? C121 C26' O103 123(2) . . ? H1W1 O1W H1W2 98.5 . . ? H2W1 O2W H2W2 122.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N101 Ni11 O101 C100 -31.6(5) . . . . ? O10 Ni11 O101 C100 145.2(4) . . . . ? O11 Ni11 O101 C100 56.1(4) . . . . ? O103 Ni11 O101 C100 -133.6(4) . . . . ? N102 Ni12 O102 C119 5.4(5) . . . . ? O103 Ni12 O102 C119 104.2(4) . . . . ? O10 Ni12 O102 C119 -175.5(4) . . . . ? O12S Ni12 O102 C119 -84.9(4) . . . . ? O102 Ni12 O103 C126 -118.0(8) . . . . ? N102 Ni12 O103 C126 -26.9(8) . . . . ? O10 Ni12 O103 C126 147.5(8) . . . . ? O12S Ni12 O103 C126 128.1(11) . . . . ? N104 Ni12 O103 C126 55.3(8) . . . . ? O102 Ni12 O103 C26' -135.2(11) . . . . ? N102 Ni12 O103 C26' -44.1(11) . . . . ? O10 Ni12 O103 C26' 130.3(11) . . . . ? O12S Ni12 O103 C26' 110.9(14) . . . . ? N104 Ni12 O103 C26' 38.1(11) . . . . ? O102 Ni12 O103 Ni11 112.54(17) . . . . ? N102 Ni12 O103 Ni11 -156.33(18) . . . . ? O10 Ni12 O103 Ni11 18.07(15) . . . . ? O12S Ni12 O103 Ni11 -1.3(10) . . . . ? N104 Ni12 O103 Ni11 -74.15(17) . . . . ? O101 Ni11 O103 C126 130.6(6) . . . . ? N101 Ni11 O103 C126 39.9(7) . . . . ? O10 Ni11 O103 C126 -139.9(6) . . . . ? O11 Ni11 O103 C126 -124.7(11) . . . . ? N103 Ni11 O103 C126 -43.8(6) . . . . ? O101 Ni11 O103 C26' 126.1(11) . . . . ? N101 Ni11 O103 C26' 35.3(12) . . . . ? O10 Ni11 O103 C26' -144.4(11) . . . . ? O11 Ni11 O103 C26' -129.3(15) . . . . ? N103 Ni11 O103 C26' -48.4(12) . . . . ? O101 Ni11 O103 Ni12 -108.07(16) . . . . ? O10 Ni11 O103 Ni12 -18.59(15) . . . . ? O11 Ni11 O103 Ni12 -3.4(10) . . . . ? N103 Ni11 O103 Ni12 77.44(19) . . . . ? O101 Ni11 N101 C106 23.6(6) . . . . ? O11 Ni11 N101 C106 -64.8(6) . . . . ? O103 Ni11 N101 C106 117.9(6) . . . . ? N103 Ni11 N101 C106 -154.0(6) . . . . ? O101 Ni11 N101 C107 -167.9(14) . . . . ? O11 Ni11 N101 C107 103.7(14) . . . . ? O103 Ni11 N101 C107 -73.6(14) . . . . ? N103 Ni11 N101 C107 14.5(13) . . . . ? O101 Ni11 N101 C17' 171.1(17) . . . . ? O11 Ni11 N101 C17' 82.7(17) . . . . ? O103 Ni11 N101 C17' -94.6(17) . . . . ? N103 Ni11 N101 C17' -6.5(17) . . . . ? O102 Ni12 N102 C113 -7.6(5) . . . . ? O103 Ni12 N102 C113 -100.7(5) . . . . ? O12S Ni12 N102 C113 83.5(5) . . . . ? N104 Ni12 N102 C113 173.1(5) . . . . ? O102 Ni12 N102 C112 177.8(4) . . . . ? O103 Ni12 N102 C112 84.7(4) . . . . ? O12S Ni12 N102 C112 -91.1(4) . . . . ? N104 Ni12 N102 C112 -1.5(4) . . . . ? N101 Ni11 N103 C120 -106.3(4) . . . . ? O10 Ni11 N103 C120 77.0(4) . . . . ? O11 Ni11 N103 C120 166.0(4) . . . . ? O103 Ni11 N103 C120 -4.1(4) . . . . ? N101 Ni11 N103 C109 137.5(5) . . . . ? O10 Ni11 N103 C109 -39.2(4) . . . . ? O11 Ni11 N103 C109 49.8(4) . . . . ? O103 Ni11 N103 C109 -120.3(4) . . . . ? N101 Ni11 N103 C18' 27.9(15) . . . . ? O10 Ni11 N103 C18' -148.8(15) . . . . ? O11 Ni11 N103 C18' -59.8(15) . . . . ? O103 Ni11 N103 C18' 130.1(15) . . . . ? N101 Ni11 N103 C108 10.0(13) . . . . ? O10 Ni11 N103 C108 -166.8(13) . . . . ? O11 Ni11 N103 C108 -77.8(13) . . . . ? O103 Ni11 N103 C108 112.2(13) . . . . ? N102 Ni12 N104 C120 100.0(4) . . . . ? O103 Ni12 N104 C120 0.8(4) . . . . ? O10 Ni12 N104 C120 -79.1(4) . . . . ? O12S Ni12 N104 C120 -169.6(4) . . . . ? N102 Ni12 N104 C111 -22.2(3) . . . . ? O103 Ni12 N104 C111 -121.4(3) . . . . ? O10 Ni12 N104 C111 158.6(3) . . . . ? O12S Ni12 N104 C111 68.1(3) . . . . ? N102 Ni12 N104 C110 -142.2(4) . . . . ? O103 Ni12 N104 C110 118.6(4) . . . . ? O10 Ni12 N104 C110 38.6(4) . . . . ? O12S Ni12 N104 C110 -51.8(4) . . . . ? O101 Ni11 O10 C11 -55.6(4) . . . . ? O11 Ni11 O10 C11 32.7(4) . . . . ? O103 Ni11 O10 C11 -149.9(4) . . . . ? N103 Ni11 O10 C11 121.6(4) . . . . ? O101 Ni11 O10 Ni12 112.74(17) . . . . ? O11 Ni11 O10 Ni12 -158.89(17) . . . . ? O103 Ni11 O10 Ni12 18.49(15) . . . . ? N103 Ni11 O10 Ni12 -70.0(2) . . . . ? O102 Ni12 O10 C11 54.4(6) . . . . ? O103 Ni12 O10 C11 146.5(6) . . . . ? O12S Ni12 O10 C11 -36.8(5) . . . . ? N104 Ni12 O10 C11 -126.4(5) . . . . ? O102 Ni12 O10 Ni11 -110.83(17) . . . . ? O103 Ni12 O10 Ni11 -18.69(16) . . . . ? O12S Ni12 O10 Ni11 158.00(17) . . . . ? N104 Ni12 O10 Ni11 68.37(17) . . . . ? O101 Ni11 O11 C13 56.8(5) . . . . ? N101 Ni11 O11 C13 146.7(5) . . . . ? O10 Ni11 O11 C13 -33.4(5) . . . . ? O103 Ni11 O11 C13 -48.3(12) . . . . ? N103 Ni11 O11 C13 -129.3(5) . . . . ? O102 Ni12 O12S C12S 19.7(4) . . . . ? N102 Ni12 O12S C12S -71.0(4) . . . . ? O103 Ni12 O12S C12S 133.7(9) . . . . ? O10 Ni12 O12S C12S 114.6(4) . . . . ? N104 Ni12 O12S C12S -153.6(4) . . . . ? Ni11 O10 C11 C12 -21.5(8) . . . . ? Ni12 O10 C11 C12 176.0(4) . . . . ? Ni11 O10 C11 C10 158.4(4) . . . . ? Ni12 O10 C11 C10 -4.0(9) . . . . ? C10 C11 C12 C13 178.0(7) . . . . ? Ni11 O11 C13 C12 23.4(9) . . . . ? Ni11 O11 C13 C14 -156.8(5) . . . . ? C11 C12 C13 O11 0.8(12) . . . . ? C11 C12 C13 C14 -179.0(7) . . . . ? Ni11 O101 C100 C101 -153.2(4) . . . . ? Ni11 O101 C100 C105 27.9(8) . . . . ? O101 C100 C101 C102 -175.8(5) . . . . ? C105 C100 C101 C102 3.2(9) . . . . ? C100 C101 C102 C103 -0.7(9) . . . . ? C101 C102 C103 C104 -1.2(10) . . . . ? C101 C102 C103 Br11 177.2(5) . . . . ? Br11 C103 C104 C105 -177.9(5) . . . . ? C103 C104 C105 C106 -176.8(6) . . . . ? C103 C104 C105 C100 2.1(10) . . . . ? O101 C100 C105 C104 175.1(6) . . . . ? C101 C100 C105 C104 -3.8(9) . . . . ? O101 C100 C105 C106 -6.1(10) . . . . ? C101 C100 C105 C106 175.0(6) . . . . ? C107 N101 C106 C105 179.8(15) . . . . ? Ni11 N101 C106 C105 -12.3(11) . . . . ? C104 C105 C106 N101 176.5(7) . . . . ? C100 C105 C106 N101 -2.3(12) . . . . ? C106 N101 C107 C108 133.8(10) . . . . ? Ni11 N101 C107 C108 -35.1(14) . . . . ? N101 C107 C108 N103 47.2(15) . . . . ? C120 N103 C108 C107 85.8(12) . . . . ? C109 N103 C108 C107 -159.4(10) . . . . ? Ni11 N103 C108 C107 -34.4(15) . . . . ? C120 N103 C109 C110 -33.9(6) . . . . ? C18' N103 C109 C110 -160.4(13) . . . . ? C108 N103 C109 C110 -152.1(9) . . . . ? Ni11 N103 C109 C110 88.9(5) . . . . ? C120 N104 C110 C109 22.5(6) . . . . ? C111 N104 C110 C109 143.6(5) . . . . ? Ni12 N104 C110 C109 -102.2(4) . . . . ? N103 C109 C110 N104 7.2(6) . . . . ? C120 N104 C111 C112 -81.3(6) . . . . ? C110 N104 C111 C112 162.7(5) . . . . ? Ni12 N104 C111 C112 43.2(5) . . . . ? C113 N102 C112 C111 -149.5(5) . . . . ? Ni12 N102 C112 C111 25.6(6) . . . . ? N104 C111 C112 N102 -47.6(6) . . . . ? C112 N102 C113 C114 -178.6(5) . . . . ? Ni12 N102 C113 C114 7.1(9) . . . . ? N102 C113 C114 C115 177.5(6) . . . . ? N102 C113 C114 C119 -1.5(10) . . . . ? C119 C114 C115 C116 1.0(9) . . . . ? C113 C114 C115 C116 -178.1(6) . . . . ? C114 C115 C116 C117 -1.0(9) . . . . ? C114 C115 C116 Br12 179.5(4) . . . . ? C115 C116 C117 C118 0.2(10) . . . . ? Br12 C116 C117 C118 179.7(5) . . . . ? C116 C117 C118 C119 0.7(10) . . . . ? Ni12 O102 C119 C118 177.7(4) . . . . ? Ni12 O102 C119 C114 -2.3(8) . . . . ? C117 C118 C119 O102 179.2(5) . . . . ? C117 C118 C119 C114 -0.7(9) . . . . ? C115 C114 C119 O102 180.0(5) . . . . ? C113 C114 C119 O102 -1.1(9) . . . . ? C115 C114 C119 C118 -0.1(8) . . . . ? C113 C114 C119 C118 178.8(5) . . . . ? C111 N104 C120 C121 71.0(6) . . . . ? C110 N104 C120 C121 -168.0(5) . . . . ? Ni12 N104 C120 C121 -46.1(6) . . . . ? C111 N104 C120 N103 -164.7(4) . . . . ? C110 N104 C120 N103 -43.7(5) . . . . ? Ni12 N104 C120 N103 78.3(5) . . . . ? C109 N103 C120 C121 173.4(5) . . . . ? C108 N103 C120 C121 -62.0(10) . . . . ? Ni11 N103 C120 C121 50.6(6) . . . . ? C109 N103 C120 N104 48.2(5) . . . . ? C18' N103 C120 N104 160.4(15) . . . . ? C108 N103 C120 N104 172.8(9) . . . . ? Ni11 N103 C120 N104 -74.6(5) . . . . ? N104 C120 C121 C26' 67.8(13) . . . . ? N103 C120 C121 C26' -49.1(13) . . . . ? N104 C120 C121 C122 -117.6(9) . . . . ? N103 C120 C121 C122 125.5(9) . . . . ? N104 C120 C121 C22' -134.2(10) . . . . ? N103 C120 C121 C22' 108.8(10) . . . . ? N104 C120 C121 C126 48.9(9) . . . . ? N103 C120 C121 C126 -68.1(9) . . . . ? C22' C121 C122 C123 -136(4) . . . . ? C120 C121 C122 C123 175.7(12) . . . . ? C121 C122 C123 Br13 174.6(9) . . . . ? Br13 C123 C124 C125 -178.0(11) . . . . ? C26' O103 C126 C125 -113(5) . . . . ? Ni12 O103 C126 C125 119.5(11) . . . . ? Ni11 O103 C126 C125 -127.2(12) . . . . ? Ni12 O103 C126 C121 -71.0(11) . . . . ? Ni11 O103 C126 C121 42.3(12) . . . . ? C124 C125 C126 O103 172.9(13) . . . . ? C122 C121 C126 O103 -176.2(9) . . . . ? C22' C121 C126 O103 -160.1(13) . . . . ? C120 C121 C126 O103 16.0(14) . . . . ? C122 C121 C126 C125 -6.3(15) . . . . ? C120 C121 C126 C125 -174.0(9) . . . . ? C121 C22' C23' Br3' -174.7(14) . . . . ? C120 C121 C26' C25' 166.2(15) . . . . ? C122 C121 C26' O103 161.6(14) . . . . ? C22' C121 C26' O103 -176.7(14) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O12S H12S O1W 0.69 1.94 2.610(6) 164 7_665 O1W H1W2 O101 0.86 1.85 2.698(6) 168.6 . O1W H1W1 O102 0.74 2.03 2.743(6) 163.2 . O2W H2W2 O11 0.87 2.01 2.875(16) 178.6 . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.033 _refine_diff_density_min -1.579 _refine_diff_density_rms 0.156 #END data_3.MeOH _database_code_depnum_ccdc_archive 'CCDC 606602' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H34 N4 Ni11 O8, C H4 O' _chemical_formula_sum 'C36 H38 N4 Ni11 O9' _chemical_formula_weight 788.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.899(2) _cell_length_b 11.4993(17) _cell_length_c 19.048(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.36(1) _cell_angle_gamma 90.00 _cell_volume 3305.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 120.0(1) _cell_measurement_reflns_used 1803 _cell_measurement_theta_min 2.86 _cell_measurement_theta_max 27.94 _exptl_crystal_description Prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1640 _exptl_absorpt_coefficient_mu 1.204 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.842133 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart-CCD-1000 BRUKER' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31327 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 28.35 _reflns_number_total 7984 _reflns_number_gt 6021 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER Smart' _computing_cell_refinement 'BRUKER Smart' _computing_data_reduction ? _computing_structure_solution 'SIR92 (A. Altomare et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0213P)^2^+3.3407P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7984 _refine_ls_number_parameters 477 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0599 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0770 _refine_ls_wR_factor_gt 0.0666 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni12 Ni 0.664842(18) 0.13613(2) 0.888109(15) 0.01339(7) Uani 1 1 d . . . Ni11 Ni 0.722503(18) -0.08125(2) 0.986913(15) 0.01333(7) Uani 1 1 d . . . O101 O 0.83401(10) -0.03168(14) 1.06419(9) 0.0178(3) Uani 1 1 d . . . O102 O 0.76556(10) 0.25241(14) 0.93268(9) 0.0166(3) Uani 1 1 d . . . O103 O 0.75761(10) 0.00758(13) 0.90728(8) 0.0143(3) Uani 1 1 d . . . N101 N 0.77252(12) -0.23964(16) 0.98296(10) 0.0158(4) Uani 1 1 d . . . N102 N 0.66406(12) 0.18984(17) 0.78762(10) 0.0161(4) Uani 1 1 d . . . N103 N 0.60860(12) -0.14781(16) 0.90207(10) 0.0142(4) Uani 1 1 d . . . N104 N 0.56654(12) 0.01262(16) 0.82714(10) 0.0141(4) Uani 1 1 d . . . O1W O 0.67920(12) -0.14033(16) 1.07495(9) 0.0179(3) Uani 1 1 d . . . O10 O 0.66447(10) 0.08167(13) 0.99115(8) 0.0145(3) Uani 1 1 d . . . O12 O 0.56108(10) 0.24667(14) 0.88203(9) 0.0186(3) Uani 1 1 d . . . O11 O 0.68155(11) 0.08434(14) 1.11172(8) 0.0189(3) Uani 1 1 d . . . C10 C 0.67380(14) 0.1352(2) 1.05264(12) 0.0145(4) Uani 1 1 d . . . C11 C 0.67636(15) 0.26550(19) 1.05336(12) 0.0151(5) Uani 1 1 d . . . C12 C 0.74202(15) 0.3197(2) 1.11076(12) 0.0184(5) Uani 1 1 d . . . H12 H 0.7841 0.2748 1.1450 0.022 Uiso 1 1 calc R . . C13 C 0.74498(16) 0.4399(2) 1.11706(13) 0.0218(5) Uani 1 1 d . . . H13 H 0.7903 0.4755 1.1541 0.026 Uiso 1 1 calc R . . C14 C 0.68032(16) 0.5069(2) 1.06808(13) 0.0212(5) Uani 1 1 d . . . H14 H 0.6807 0.5873 1.0734 0.025 Uiso 1 1 calc R . . C15 C 0.61489(16) 0.4536(2) 1.01103(13) 0.0201(5) Uani 1 1 d . . . H15 H 0.5714 0.4990 0.9784 0.024 Uiso 1 1 calc R . . C16 C 0.61320(14) 0.3331(2) 1.00180(12) 0.0159(5) Uani 1 1 d . . . C17 C 0.54056(15) 0.28105(19) 0.93785(12) 0.0161(5) Uani 1 1 d . . . O13 O 0.46475(10) 0.27903(15) 0.94339(9) 0.0220(4) Uani 1 1 d . . . C100 C 0.89256(14) -0.1013(2) 1.10913(12) 0.0168(5) Uani 1 1 d . . . C101 C 0.95361(16) -0.0560(2) 1.17341(13) 0.0229(5) Uani 1 1 d . . . H101 H 0.9504 0.0223 1.1844 0.027 Uiso 1 1 calc R . . C102 C 1.01840(16) -0.1240(2) 1.22086(14) 0.0285(6) Uani 1 1 d . . . H102 H 1.0578 -0.0908 1.2629 0.034 Uiso 1 1 calc R . . C103 C 1.02554(16) -0.2413(2) 1.20667(14) 0.0274(6) Uani 1 1 d . . . H103 H 1.0703 -0.2864 1.2380 0.033 Uiso 1 1 calc R . . C104 C 0.96502(15) -0.2894(2) 1.14516(14) 0.0227(5) Uani 1 1 d . . . H104 H 0.9688 -0.3684 1.1360 0.027 Uiso 1 1 calc R . . C105 C 0.89742(14) -0.2229(2) 1.09556(13) 0.0177(5) Uani 1 1 d . . . C106 C 0.83776(15) -0.2843(2) 1.03382(13) 0.0186(5) Uani 1 1 d . . . H106 H 0.8475 -0.3636 1.0306 0.022 Uiso 1 1 calc R . . C107 C 0.71516(15) -0.3142(2) 0.92491(13) 0.0191(5) Uani 1 1 d . . . H10A H 0.7222 -0.3949 0.9405 0.023 Uiso 1 1 calc R . . H10B H 0.7308 -0.3069 0.8798 0.023 Uiso 1 1 calc R . . C108 C 0.61967(15) -0.27569(19) 0.91126(13) 0.0169(5) Uani 1 1 d . . . H10C H 0.5820 -0.3138 0.8671 0.020 Uiso 1 1 calc R . . H10D H 0.6006 -0.3002 0.9526 0.020 Uiso 1 1 calc R . . C109 C 0.52291(14) -0.1088(2) 0.91130(12) 0.0168(5) Uani 1 1 d . . . H10E H 0.5316 -0.0841 0.9618 0.020 Uiso 1 1 calc R . . H10F H 0.4796 -0.1711 0.8991 0.020 Uiso 1 1 calc R . . C110 C 0.49237(15) -0.0069(2) 0.85774(13) 0.0181(5) Uani 1 1 d . . . H11A H 0.4382 -0.0262 0.8187 0.022 Uiso 1 1 calc R . . H11B H 0.4821 0.0618 0.8835 0.022 Uiso 1 1 calc R . . C111 C 0.53269(15) 0.0665(2) 0.75286(12) 0.0184(5) Uani 1 1 d . . . H11C H 0.4910 0.1276 0.7539 0.022 Uiso 1 1 calc R . . H11D H 0.5012 0.0084 0.7174 0.022 Uiso 1 1 calc R . . C112 C 0.60704(15) 0.1176(2) 0.72786(12) 0.0180(5) Uani 1 1 d . . . H11E H 0.6416 0.0554 0.7161 0.022 Uiso 1 1 calc R . . H11F H 0.5822 0.1644 0.6838 0.022 Uiso 1 1 calc R . . C113 C 0.69836(15) 0.2820(2) 0.77102(12) 0.0173(5) Uani 1 1 d . . . H113 H 0.6823 0.3015 0.7212 0.021 Uiso 1 1 calc R . . C114 C 0.76066(15) 0.3601(2) 0.82297(12) 0.0175(5) Uani 1 1 d . . . C115 C 0.79277(16) 0.4546(2) 0.79247(14) 0.0222(5) Uani 1 1 d . . . H115 H 0.7702 0.4682 0.7419 0.027 Uiso 1 1 calc R . . C116 C 0.85715(17) 0.5278(2) 0.83585(14) 0.0245(5) Uani 1 1 d . . . H116 H 0.8780 0.5896 0.8145 0.029 Uiso 1 1 calc R . . C117 C 0.89034(16) 0.5087(2) 0.91122(14) 0.0225(5) Uani 1 1 d . . . H117 H 0.9342 0.5573 0.9405 0.027 Uiso 1 1 calc R . . C118 C 0.85877(15) 0.4173(2) 0.94350(13) 0.0201(5) Uani 1 1 d . . . H118 H 0.8808 0.4061 0.9944 0.024 Uiso 1 1 calc R . . C119 C 0.79430(15) 0.34228(19) 0.90021(13) 0.0170(5) Uani 1 1 d . . . C120 C 0.60055(15) -0.10777(19) 0.82557(12) 0.0151(5) Uani 1 1 d . . . H120 H 0.5546 -0.1539 0.7901 0.018 Uiso 1 1 calc R . . C121 C 0.68458(14) -0.11704(19) 0.80621(12) 0.0150(4) Uani 1 1 d . . . C122 C 0.68796(16) -0.1857(2) 0.74682(13) 0.0186(5) Uani 1 1 d . . . H122 H 0.6370 -0.2229 0.7177 0.022 Uiso 1 1 calc R . . C123 C 0.76644(16) -0.1991(2) 0.73081(13) 0.0208(5) Uani 1 1 d . . . H123 H 0.7689 -0.2460 0.6917 0.025 Uiso 1 1 calc R . . C124 C 0.84169(16) -0.1411(2) 0.77415(13) 0.0216(5) Uani 1 1 d . . . H124 H 0.8948 -0.1500 0.7640 0.026 Uiso 1 1 calc R . . C125 C 0.83872(15) -0.0705(2) 0.83206(13) 0.0187(5) Uani 1 1 d . . . H125 H 0.8894 -0.0309 0.8595 0.022 Uiso 1 1 calc R . . C126 C 0.76023(15) -0.05795(19) 0.84972(12) 0.0149(4) Uani 1 1 d . . . H2 H 0.812(2) 0.228(3) 0.978(2) 0.063(11) Uiso 1 1 d . . . H1WA H 0.6789(19) -0.073(3) 1.0973(16) 0.034(8) Uiso 1 1 d . . . H1WB H 0.6390(19) -0.176(3) 1.0712(16) 0.028(9) Uiso 1 1 d . . . O1S O 0.88419(11) 0.17277(16) 1.04036(10) 0.0230(4) Uani 1 1 d . . . C1S C 0.95811(18) 0.1545(3) 1.01342(18) 0.0384(7) Uani 1 1 d . . . H1S1 H 0.9993 0.2176 1.0290 0.058 Uiso 1 1 calc R . . H1S2 H 0.9374 0.1509 0.9604 0.058 Uiso 1 1 calc R . . H1S3 H 0.9870 0.0827 1.0329 0.058 Uiso 1 1 calc R . . H1S H 0.868(2) 0.104(3) 1.0514(18) 0.055(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni12 0.01568(14) 0.01385(14) 0.01095(13) 0.00102(11) 0.00465(11) 0.00078(12) Ni11 0.01550(14) 0.01224(14) 0.01230(14) 0.00044(11) 0.00444(11) 0.00054(11) O101 0.0176(8) 0.0148(8) 0.0189(8) 0.0023(7) 0.0028(7) -0.0001(6) O102 0.0187(8) 0.0161(8) 0.0148(8) 0.0040(7) 0.0048(7) -0.0017(7) O103 0.0166(8) 0.0148(8) 0.0120(7) -0.0011(6) 0.0049(6) 0.0000(6) N101 0.0183(10) 0.0143(9) 0.0161(9) -0.0013(8) 0.0073(8) 0.0007(8) N102 0.0175(9) 0.0174(10) 0.0133(9) 0.0011(8) 0.0049(8) 0.0021(8) N103 0.0165(9) 0.0142(9) 0.0128(9) 0.0006(8) 0.0059(7) 0.0000(8) N104 0.0155(9) 0.0146(9) 0.0125(9) 0.0026(7) 0.0049(7) 0.0010(8) O1W 0.0221(9) 0.0154(9) 0.0172(8) 0.0003(7) 0.0073(7) -0.0025(8) O10 0.0184(8) 0.0127(7) 0.0127(7) -0.0009(6) 0.0055(6) 0.0014(6) O12 0.0207(8) 0.0194(8) 0.0156(8) -0.0003(7) 0.0055(7) 0.0051(7) O11 0.0272(9) 0.0173(8) 0.0134(8) 0.0011(7) 0.0079(7) 0.0016(7) C10 0.0129(10) 0.0165(11) 0.0146(11) 0.0001(9) 0.0051(8) 0.0013(9) C11 0.0203(11) 0.0138(11) 0.0140(11) -0.0004(9) 0.0094(9) 0.0018(9) C12 0.0201(11) 0.0219(12) 0.0129(11) -0.0004(9) 0.0049(9) 0.0015(10) C13 0.0243(12) 0.0214(13) 0.0196(12) -0.0059(10) 0.0065(10) -0.0041(10) C14 0.0287(13) 0.0131(11) 0.0247(13) -0.0027(10) 0.0124(11) -0.0019(10) C15 0.0222(12) 0.0173(12) 0.0214(12) 0.0029(10) 0.0078(10) 0.0024(10) C16 0.0173(11) 0.0170(11) 0.0155(11) 0.0001(9) 0.0084(9) -0.0005(9) C17 0.0196(11) 0.0111(10) 0.0165(11) 0.0035(9) 0.0040(9) 0.0036(9) O13 0.0181(8) 0.0246(9) 0.0246(9) -0.0025(7) 0.0088(7) -0.0027(7) C100 0.0141(10) 0.0210(12) 0.0170(11) 0.0047(9) 0.0073(9) -0.0010(9) C101 0.0220(12) 0.0226(13) 0.0221(12) 0.0017(10) 0.0041(10) -0.0042(10) C102 0.0216(12) 0.0363(15) 0.0216(13) 0.0048(12) -0.0018(10) -0.0081(11) C103 0.0172(12) 0.0342(15) 0.0278(14) 0.0111(12) 0.0027(10) 0.0030(11) C104 0.0209(12) 0.0225(13) 0.0259(13) 0.0059(11) 0.0089(10) 0.0047(10) C105 0.0162(11) 0.0208(12) 0.0186(11) 0.0053(10) 0.0091(9) 0.0017(9) C106 0.0210(12) 0.0169(11) 0.0207(12) 0.0022(10) 0.0106(10) 0.0039(10) C107 0.0265(13) 0.0121(11) 0.0191(12) -0.0012(9) 0.0076(10) 0.0011(10) C108 0.0192(11) 0.0135(11) 0.0175(11) -0.0008(9) 0.0051(9) -0.0013(9) C109 0.0144(10) 0.0204(12) 0.0164(11) 0.0002(9) 0.0062(9) -0.0006(9) C110 0.0165(11) 0.0199(12) 0.0187(12) 0.0032(10) 0.0069(9) -0.0009(9) C111 0.0187(11) 0.0207(12) 0.0132(11) 0.0032(9) 0.0013(9) -0.0007(10) C112 0.0216(11) 0.0200(12) 0.0120(11) 0.0032(9) 0.0047(9) 0.0000(9) C113 0.0194(11) 0.0203(12) 0.0129(11) 0.0021(9) 0.0060(9) 0.0035(9) C114 0.0215(11) 0.0160(11) 0.0167(11) 0.0015(9) 0.0087(9) 0.0020(10) C115 0.0273(13) 0.0216(12) 0.0196(12) 0.0038(10) 0.0100(10) 0.0006(10) C116 0.0307(14) 0.0166(12) 0.0300(14) 0.0028(11) 0.0153(11) -0.0021(10) C117 0.0223(12) 0.0182(12) 0.0274(13) -0.0023(10) 0.0085(10) -0.0014(10) C118 0.0223(12) 0.0186(12) 0.0194(12) -0.0015(10) 0.0066(10) -0.0008(10) C119 0.0198(11) 0.0142(11) 0.0197(11) 0.0013(9) 0.0101(9) 0.0029(9) C120 0.0176(11) 0.0133(11) 0.0132(10) -0.0024(9) 0.0032(9) -0.0019(9) C121 0.0173(11) 0.0152(11) 0.0134(10) 0.0011(9) 0.0062(9) 0.0023(9) C122 0.0236(12) 0.0164(11) 0.0159(11) -0.0007(9) 0.0064(10) -0.0012(10) C123 0.0305(13) 0.0181(12) 0.0161(11) -0.0009(10) 0.0106(10) 0.0027(10) C124 0.0227(12) 0.0245(13) 0.0220(12) 0.0015(10) 0.0133(10) 0.0051(10) C125 0.0181(11) 0.0217(12) 0.0173(11) 0.0007(10) 0.0072(9) -0.0007(10) C126 0.0199(11) 0.0134(11) 0.0121(10) 0.0026(9) 0.0062(9) 0.0017(9) O1S 0.0225(9) 0.0195(9) 0.0236(9) 0.0051(7) 0.0026(7) -0.0008(7) C1S 0.0238(14) 0.0322(16) 0.060(2) 0.0123(15) 0.0135(14) 0.0045(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni12 N102 2.0076(19) . ? Ni12 O103 2.0383(15) . ? Ni12 O102 2.0534(16) . ? Ni12 O12 2.0568(16) . ? Ni12 O10 2.0620(15) . ? Ni12 N104 2.1599(19) . ? Ni11 O101 1.9976(16) . ? Ni11 N101 1.9983(19) . ? Ni11 O103 2.0468(15) . ? Ni11 O10 2.1011(15) . ? Ni11 O1W 2.1154(17) . ? Ni11 N103 2.1525(18) . ? O101 C100 1.319(3) . ? O102 C119 1.356(3) . ? O102 H2 0.99(4) . ? O103 C126 1.342(3) . ? N101 C106 1.283(3) . ? N101 C107 1.468(3) . ? N102 C113 1.276(3) . ? N102 C112 1.469(3) . ? N103 C108 1.485(3) . ? N103 C120 1.495(3) . ? N103 C109 1.496(3) . ? N104 C111 1.482(3) . ? N104 C110 1.488(3) . ? N104 C120 1.490(3) . ? O1W H1WA 0.89(3) . ? O1W H1WB 0.74(3) . ? O10 C10 1.290(3) . ? O12 C17 1.270(3) . ? O11 C10 1.239(3) . ? C10 C11 1.499(3) . ? C11 C12 1.398(3) . ? C11 C16 1.398(3) . ? C12 C13 1.387(3) . ? C12 H12 0.9300 . ? C13 C14 1.384(3) . ? C13 H13 0.9300 . ? C14 C15 1.388(3) . ? C14 H14 0.9300 . ? C15 C16 1.397(3) . ? C15 H15 0.9300 . ? C16 C17 1.513(3) . ? C17 O13 1.243(3) . ? C100 C101 1.402(3) . ? C100 C105 1.427(3) . ? C101 C102 1.380(3) . ? C101 H101 0.9300 . ? C102 C103 1.387(4) . ? C102 H102 0.9300 . ? C103 C104 1.377(4) . ? C103 H103 0.9300 . ? C104 C105 1.412(3) . ? C104 H104 0.9300 . ? C105 C106 1.442(3) . ? C106 H106 0.9300 . ? C107 C108 1.523(3) . ? C107 H10A 0.9700 . ? C107 H10B 0.9700 . ? C108 H10C 0.9700 . ? C108 H10D 0.9700 . ? C109 C110 1.529(3) . ? C109 H10E 0.9700 . ? C109 H10F 0.9700 . ? C110 H11A 0.9700 . ? C110 H11B 0.9700 . ? C111 C112 1.524(3) . ? C111 H11C 0.9700 . ? C111 H11D 0.9700 . ? C112 H11E 0.9700 . ? C112 H11F 0.9700 . ? C113 C114 1.466(3) . ? C113 H113 0.9300 . ? C114 C115 1.402(3) . ? C114 C119 1.413(3) . ? C115 C116 1.381(4) . ? C115 H115 0.9300 . ? C116 C117 1.382(3) . ? C116 H116 0.9300 . ? C117 C118 1.389(3) . ? C117 H117 0.9300 . ? C118 C119 1.394(3) . ? C118 H118 0.9300 . ? C120 C121 1.498(3) . ? C120 H120 0.9800 . ? C121 C122 1.394(3) . ? C121 C126 1.403(3) . ? C122 C123 1.383(3) . ? C122 H122 0.9300 . ? C123 C124 1.391(3) . ? C123 H123 0.9300 . ? C124 C125 1.383(3) . ? C124 H124 0.9300 . ? C125 C126 1.398(3) . ? C125 H125 0.9300 . ? O1S C1S 1.438(3) . ? O1S H1S 0.87(4) . ? C1S H1S1 0.9600 . ? C1S H1S2 0.9600 . ? C1S H1S3 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N102 Ni12 O103 100.41(7) . . ? N102 Ni12 O102 87.92(7) . . ? O103 Ni12 O102 88.40(6) . . ? N102 Ni12 O12 89.55(7) . . ? O103 Ni12 O12 168.70(6) . . ? O102 Ni12 O12 97.36(7) . . ? N102 Ni12 O10 179.45(7) . . ? O103 Ni12 O10 80.10(6) . . ? O102 Ni12 O10 92.28(6) . . ? O12 Ni12 O10 89.92(6) . . ? N102 Ni12 N104 84.47(7) . . ? O103 Ni12 N104 88.83(7) . . ? O102 Ni12 N104 171.30(7) . . ? O12 Ni12 N104 86.81(7) . . ? O10 Ni12 N104 95.37(6) . . ? O101 Ni11 N101 90.95(7) . . ? O101 Ni11 O103 91.02(6) . . ? N101 Ni11 O103 102.84(7) . . ? O101 Ni11 O10 90.91(6) . . ? N101 Ni11 O10 177.37(7) . . ? O103 Ni11 O10 78.99(6) . . ? O101 Ni11 O1W 86.70(7) . . ? N101 Ni11 O1W 88.27(7) . . ? O103 Ni11 O1W 168.70(7) . . ? O10 Ni11 O1W 89.97(6) . . ? O101 Ni11 N103 174.98(7) . . ? N101 Ni11 N103 84.16(7) . . ? O103 Ni11 N103 88.99(6) . . ? O10 Ni11 N103 94.02(6) . . ? O1W Ni11 N103 94.24(7) . . ? C100 O101 Ni11 125.88(14) . . ? C119 O102 Ni12 129.71(14) . . ? C119 O102 H2 111(2) . . ? Ni12 O102 H2 116(2) . . ? C126 O103 Ni12 117.90(13) . . ? C126 O103 Ni11 114.28(13) . . ? Ni12 O103 Ni11 98.27(6) . . ? C106 N101 C107 119.8(2) . . ? C106 N101 Ni11 124.98(16) . . ? C107 N101 Ni11 113.63(14) . . ? C113 N102 C112 119.03(19) . . ? C113 N102 Ni12 128.08(16) . . ? C112 N102 Ni12 112.45(14) . . ? C108 N103 C120 112.98(17) . . ? C108 N103 C109 111.20(17) . . ? C120 N103 C109 102.75(16) . . ? C108 N103 Ni11 102.90(13) . . ? C120 N103 Ni11 114.57(13) . . ? C109 N103 Ni11 112.77(13) . . ? C111 N104 C110 110.05(17) . . ? C111 N104 C120 113.22(17) . . ? C110 N104 C120 101.84(16) . . ? C111 N104 Ni12 102.82(13) . . ? C110 N104 Ni12 114.66(14) . . ? C120 N104 Ni12 114.58(13) . . ? Ni11 O1W H1WA 98.7(19) . . ? Ni11 O1W H1WB 126(2) . . ? H1WA O1W H1WB 113(3) . . ? C10 O10 Ni12 133.27(14) . . ? C10 O10 Ni11 122.29(14) . . ? Ni12 O10 Ni11 95.81(6) . . ? C17 O12 Ni12 123.95(14) . . ? O11 C10 O10 123.3(2) . . ? O11 C10 C11 118.0(2) . . ? O10 C10 C11 118.72(19) . . ? C12 C11 C16 119.7(2) . . ? C12 C11 C10 117.7(2) . . ? C16 C11 C10 122.5(2) . . ? C13 C12 C11 120.6(2) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C14 C13 C12 119.9(2) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C13 C14 C15 119.8(2) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C14 C15 C16 121.1(2) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C15 C16 C11 118.8(2) . . ? C15 C16 C17 118.3(2) . . ? C11 C16 C17 122.9(2) . . ? O13 C17 O12 125.3(2) . . ? O13 C17 C16 117.0(2) . . ? O12 C17 C16 117.71(19) . . ? O101 C100 C101 119.6(2) . . ? O101 C100 C105 123.0(2) . . ? C101 C100 C105 117.4(2) . . ? C102 C101 C100 122.0(2) . . ? C102 C101 H101 119.0 . . ? C100 C101 H101 119.0 . . ? C101 C102 C103 120.9(2) . . ? C101 C102 H102 119.5 . . ? C103 C102 H102 119.5 . . ? C104 C103 C102 118.6(2) . . ? C104 C103 H103 120.7 . . ? C102 C103 H103 120.7 . . ? C103 C104 C105 122.1(2) . . ? C103 C104 H104 118.9 . . ? C105 C104 H104 118.9 . . ? C104 C105 C100 118.9(2) . . ? C104 C105 C106 116.5(2) . . ? C100 C105 C106 124.6(2) . . ? N101 C106 C105 126.0(2) . . ? N101 C106 H106 117.0 . . ? C105 C106 H106 117.0 . . ? N101 C107 C108 107.94(18) . . ? N101 C107 H10A 110.1 . . ? C108 C107 H10A 110.1 . . ? N101 C107 H10B 110.1 . . ? C108 C107 H10B 110.1 . . ? H10A C107 H10B 108.4 . . ? N103 C108 C107 112.52(18) . . ? N103 C108 H10C 109.1 . . ? C107 C108 H10C 109.1 . . ? N103 C108 H10D 109.1 . . ? C107 C108 H10D 109.1 . . ? H10C C108 H10D 107.8 . . ? N103 C109 C110 105.13(17) . . ? N103 C109 H10E 110.7 . . ? C110 C109 H10E 110.7 . . ? N103 C109 H10F 110.7 . . ? C110 C109 H10F 110.7 . . ? H10E C109 H10F 108.8 . . ? N104 C110 C109 104.64(17) . . ? N104 C110 H11A 110.8 . . ? C109 C110 H11A 110.8 . . ? N104 C110 H11B 110.8 . . ? C109 C110 H11B 110.8 . . ? H11A C110 H11B 108.9 . . ? N104 C111 C112 112.04(18) . . ? N104 C111 H11C 109.2 . . ? C112 C111 H11C 109.2 . . ? N104 C111 H11D 109.2 . . ? C112 C111 H11D 109.2 . . ? H11C C111 H11D 107.9 . . ? N102 C112 C111 109.02(18) . . ? N102 C112 H11E 109.9 . . ? C111 C112 H11E 109.9 . . ? N102 C112 H11F 109.9 . . ? C111 C112 H11F 109.9 . . ? H11E C112 H11F 108.3 . . ? N102 C113 C114 126.3(2) . . ? N102 C113 H113 116.9 . . ? C114 C113 H113 116.9 . . ? C115 C114 C119 118.4(2) . . ? C115 C114 C113 116.9(2) . . ? C119 C114 C113 124.6(2) . . ? C116 C115 C114 121.5(2) . . ? C116 C115 H115 119.2 . . ? C114 C115 H115 119.2 . . ? C115 C116 C117 119.5(2) . . ? C115 C116 H116 120.2 . . ? C117 C116 H116 120.2 . . ? C116 C117 C118 120.5(2) . . ? C116 C117 H117 119.7 . . ? C118 C117 H117 119.7 . . ? C117 C118 C119 120.5(2) . . ? C117 C118 H118 119.8 . . ? C119 C118 H118 119.8 . . ? O102 C119 C118 119.5(2) . . ? O102 C119 C114 120.9(2) . . ? C118 C119 C114 119.5(2) . . ? N104 C120 N103 100.76(16) . . ? N104 C120 C121 115.39(18) . . ? N103 C120 C121 114.15(18) . . ? N104 C120 H120 108.7 . . ? N103 C120 H120 108.7 . . ? C121 C120 H120 108.7 . . ? C122 C121 C126 120.6(2) . . ? C122 C121 C120 120.4(2) . . ? C126 C121 C120 119.04(19) . . ? C123 C122 C121 120.6(2) . . ? C123 C122 H122 119.7 . . ? C121 C122 H122 119.7 . . ? C122 C123 C124 118.9(2) . . ? C122 C123 H123 120.6 . . ? C124 C123 H123 120.6 . . ? C125 C124 C123 121.0(2) . . ? C125 C124 H124 119.5 . . ? C123 C124 H124 119.5 . . ? C124 C125 C126 120.6(2) . . ? C124 C125 H125 119.7 . . ? C126 C125 H125 119.7 . . ? O103 C126 C125 120.9(2) . . ? O103 C126 C121 120.88(19) . . ? C125 C126 C121 118.2(2) . . ? C1S O1S H1S 107(2) . . ? O1S C1S H1S1 109.5 . . ? O1S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? O1S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N101 Ni11 O101 C100 -22.79(18) . . . . ? O103 Ni11 O101 C100 -125.65(17) . . . . ? O10 Ni11 O101 C100 155.34(17) . . . . ? O1W Ni11 O101 C100 65.43(17) . . . . ? N102 Ni12 O102 C119 14.39(18) . . . . ? O103 Ni12 O102 C119 114.87(18) . . . . ? O12 Ni12 O102 C119 -74.89(18) . . . . ? O10 Ni12 O102 C119 -165.10(18) . . . . ? N102 Ni12 O103 C126 -36.54(16) . . . . ? O102 Ni12 O103 C126 -124.13(15) . . . . ? O12 Ni12 O103 C126 114.9(3) . . . . ? O10 Ni12 O103 C126 143.27(15) . . . . ? N104 Ni12 O103 C126 47.62(15) . . . . ? N102 Ni12 O103 Ni11 -159.71(7) . . . . ? O102 Ni12 O103 Ni11 112.70(6) . . . . ? O12 Ni12 O103 Ni11 -8.2(3) . . . . ? O10 Ni12 O103 Ni11 20.10(6) . . . . ? N104 Ni12 O103 Ni11 -75.55(7) . . . . ? O101 Ni11 O103 C126 123.74(14) . . . . ? N101 Ni11 O103 C126 32.53(15) . . . . ? O10 Ni11 O103 C126 -145.54(15) . . . . ? O1W Ni11 O103 C126 -158.1(3) . . . . ? N103 Ni11 O103 C126 -51.25(14) . . . . ? O101 Ni11 O103 Ni12 -110.51(7) . . . . ? N101 Ni11 O103 Ni12 158.29(7) . . . . ? O10 Ni11 O103 Ni12 -19.78(6) . . . . ? O1W Ni11 O103 Ni12 -32.3(4) . . . . ? N103 Ni11 O103 Ni12 74.51(7) . . . . ? O101 Ni11 N101 C106 19.86(19) . . . . ? O103 Ni11 N101 C106 111.12(19) . . . . ? O1W Ni11 N101 C106 -66.81(19) . . . . ? N103 Ni11 N101 C106 -161.26(19) . . . . ? O101 Ni11 N101 C107 -174.45(15) . . . . ? O103 Ni11 N101 C107 -83.18(15) . . . . ? O1W Ni11 N101 C107 98.89(15) . . . . ? N103 Ni11 N101 C107 4.44(15) . . . . ? O103 Ni12 N102 C113 -104.5(2) . . . . ? O102 Ni12 N102 C113 -16.5(2) . . . . ? O12 Ni12 N102 C113 80.9(2) . . . . ? N104 Ni12 N102 C113 167.7(2) . . . . ? O103 Ni12 N102 C112 83.35(15) . . . . ? O102 Ni12 N102 C112 171.34(15) . . . . ? O12 Ni12 N102 C112 -91.28(15) . . . . ? N104 Ni12 N102 C112 -4.44(15) . . . . ? N101 Ni11 N103 C108 20.32(13) . . . . ? O103 Ni11 N103 C108 123.34(13) . . . . ? O10 Ni11 N103 C108 -157.77(13) . . . . ? O1W Ni11 N103 C108 -67.51(13) . . . . ? N101 Ni11 N103 C120 -102.71(15) . . . . ? O103 Ni11 N103 C120 0.30(14) . . . . ? O10 Ni11 N103 C120 79.20(14) . . . . ? O1W Ni11 N103 C120 169.46(14) . . . . ? N101 Ni11 N103 C109 140.22(15) . . . . ? O103 Ni11 N103 C109 -116.76(14) . . . . ? O10 Ni11 N103 C109 -37.87(14) . . . . ? O1W Ni11 N103 C109 52.39(14) . . . . ? O103 Ni12 N104 C111 -121.10(13) . . . . ? O12 Ni12 N104 C111 69.34(13) . . . . ? O10 Ni12 N104 C111 158.96(13) . . . . ? N102 Ni12 N104 C110 -139.95(15) . . . . ? O103 Ni12 N104 C110 119.47(14) . . . . ? O102 Ni12 N104 C110 -169.0(4) . . . . ? O12 Ni12 N104 C110 -50.09(14) . . . . ? O10 Ni12 N104 C110 39.52(15) . . . . ? N102 Ni12 N104 C120 102.77(14) . . . . ? O103 Ni12 N104 C120 2.19(14) . . . . ? O12 Ni12 N104 C120 -167.37(14) . . . . ? O10 Ni12 N104 C120 -77.76(14) . . . . ? O103 Ni12 O10 C10 126.99(19) . . . . ? O102 Ni12 O10 C10 39.01(19) . . . . ? O12 Ni12 O10 C10 -58.35(19) . . . . ? N104 Ni12 O10 C10 -145.14(19) . . . . ? O103 Ni12 O10 Ni11 -19.45(6) . . . . ? O102 Ni12 O10 Ni11 -107.43(6) . . . . ? O12 Ni12 O10 Ni11 155.21(6) . . . . ? N104 Ni12 O10 Ni11 68.42(7) . . . . ? O101 Ni11 O10 C10 -41.27(16) . . . . ? O103 Ni11 O10 C10 -132.13(16) . . . . ? O1W Ni11 O10 C10 45.43(16) . . . . ? N103 Ni11 O10 C10 139.68(16) . . . . ? O101 Ni11 O10 Ni12 110.30(7) . . . . ? O103 Ni11 O10 Ni12 19.44(6) . . . . ? O1W Ni11 O10 Ni12 -163.00(7) . . . . ? N103 Ni11 O10 Ni12 -68.75(7) . . . . ? N102 Ni12 O12 C17 -160.31(18) . . . . ? O103 Ni12 O12 C17 47.7(4) . . . . ? O102 Ni12 O12 C17 -72.46(18) . . . . ? O10 Ni12 O12 C17 19.83(18) . . . . ? N104 Ni12 O12 C17 115.21(18) . . . . ? Ni12 O10 C10 O11 -171.48(15) . . . . ? Ni11 O10 C10 O11 -32.1(3) . . . . ? Ni12 O10 C10 C11 7.9(3) . . . . ? Ni11 O10 C10 C11 147.33(15) . . . . ? O11 C10 C11 C12 45.0(3) . . . . ? O10 C10 C11 C12 -134.4(2) . . . . ? O11 C10 C11 C16 -131.3(2) . . . . ? O10 C10 C11 C16 49.2(3) . . . . ? C16 C11 C12 C13 0.1(3) . . . . ? C10 C11 C12 C13 -176.3(2) . . . . ? C11 C12 C13 C14 2.7(4) . . . . ? C12 C13 C14 C15 -2.6(4) . . . . ? C13 C14 C15 C16 -0.3(4) . . . . ? C14 C15 C16 C11 3.1(3) . . . . ? C14 C15 C16 C17 -179.3(2) . . . . ? C12 C11 C16 C15 -3.0(3) . . . . ? C10 C11 C16 C15 173.3(2) . . . . ? C12 C11 C16 C17 179.5(2) . . . . ? C10 C11 C16 C17 -4.2(3) . . . . ? Ni12 O12 C17 O13 -130.9(2) . . . . ? Ni12 O12 C17 C16 51.6(3) . . . . ? C15 C16 C17 O13 -73.2(3) . . . . ? C11 C16 C17 O13 104.3(3) . . . . ? C15 C16 C17 O12 104.5(2) . . . . ? C11 C16 C17 O12 -78.0(3) . . . . ? Ni11 O101 C100 C101 -161.99(16) . . . . ? Ni11 O101 C100 C105 18.1(3) . . . . ? O101 C100 C101 C102 -177.5(2) . . . . ? C105 C100 C101 C102 2.4(3) . . . . ? C100 C101 C102 C103 -0.1(4) . . . . ? C101 C102 C103 C104 -1.8(4) . . . . ? C102 C103 C104 C105 1.3(4) . . . . ? C103 C104 C105 C100 0.9(3) . . . . ? C103 C104 C105 C106 -179.3(2) . . . . ? O101 C100 C105 C104 177.1(2) . . . . ? C101 C100 C105 C104 -2.7(3) . . . . ? O101 C100 C105 C106 -2.6(3) . . . . ? C101 C100 C105 C106 177.5(2) . . . . ? C107 N101 C106 C105 -177.6(2) . . . . ? Ni11 N101 C106 C105 -12.7(3) . . . . ? C104 C105 C106 N101 -179.9(2) . . . . ? C100 C105 C106 N101 -0.2(4) . . . . ? C106 N101 C107 C108 138.4(2) . . . . ? Ni11 N101 C107 C108 -28.1(2) . . . . ? C120 N103 C108 C107 82.0(2) . . . . ? C109 N103 C108 C107 -163.10(18) . . . . ? Ni11 N103 C108 C107 -42.1(2) . . . . ? N101 C107 C108 N103 48.2(2) . . . . ? C108 N103 C109 C110 -145.78(18) . . . . ? C120 N103 C109 C110 -24.6(2) . . . . ? Ni11 N103 C109 C110 99.23(17) . . . . ? C111 N104 C110 C109 153.66(18) . . . . ? C120 N104 C110 C109 33.3(2) . . . . ? Ni12 N104 C110 C109 -91.03(18) . . . . ? N103 C109 C110 N104 -5.3(2) . . . . ? C110 N104 C111 C112 164.77(19) . . . . ? C120 N104 C111 C112 -82.0(2) . . . . ? Ni12 N104 C111 C112 42.2(2) . . . . ? C113 N102 C112 C111 -144.5(2) . . . . ? Ni12 N102 C112 C111 28.5(2) . . . . ? N104 C111 C112 N102 -49.0(3) . . . . ? C112 N102 C113 C114 -176.1(2) . . . . ? Ni12 N102 C113 C114 12.2(3) . . . . ? N102 C113 C114 C115 177.7(2) . . . . ? N102 C113 C114 C119 2.0(4) . . . . ? C119 C114 C115 C116 1.4(4) . . . . ? C113 C114 C115 C116 -174.6(2) . . . . ? C114 C115 C116 C117 -0.6(4) . . . . ? C115 C116 C117 C118 -0.7(4) . . . . ? C116 C117 C118 C119 1.2(4) . . . . ? Ni12 O102 C119 C118 173.65(16) . . . . ? Ni12 O102 C119 C114 -7.2(3) . . . . ? C117 C118 C119 O102 178.8(2) . . . . ? C117 C118 C119 C114 -0.4(3) . . . . ? C115 C114 C119 O102 179.9(2) . . . . ? C113 C114 C119 O102 -4.4(3) . . . . ? C115 C114 C119 C118 -0.9(3) . . . . ? C113 C114 C119 C118 174.8(2) . . . . ? C111 N104 C120 N103 -167.04(16) . . . . ? C110 N104 C120 N103 -48.93(19) . . . . ? Ni12 N104 C120 N103 75.45(16) . . . . ? C111 N104 C120 C121 69.5(2) . . . . ? C110 N104 C120 C121 -172.38(18) . . . . ? Ni12 N104 C120 C121 -48.0(2) . . . . ? C108 N103 C120 N104 165.40(17) . . . . ? C109 N103 C120 N104 45.48(19) . . . . ? Ni11 N103 C120 N104 -77.18(16) . . . . ? C108 N103 C120 C121 -70.3(2) . . . . ? C109 N103 C120 C121 169.78(18) . . . . ? Ni11 N103 C120 C121 47.1(2) . . . . ? N104 C120 C121 C122 -123.7(2) . . . . ? N103 C120 C121 C122 120.2(2) . . . . ? N104 C120 C121 C126 57.8(3) . . . . ? N103 C120 C121 C126 -58.3(3) . . . . ? C126 C121 C122 C123 1.6(3) . . . . ? C120 C121 C122 C123 -176.9(2) . . . . ? C121 C122 C123 C124 -1.2(4) . . . . ? C122 C123 C124 C125 -0.4(4) . . . . ? C123 C124 C125 C126 1.7(4) . . . . ? Ni12 O103 C126 C125 125.59(19) . . . . ? Ni11 O103 C126 C125 -119.74(19) . . . . ? Ni12 O103 C126 C121 -55.3(2) . . . . ? Ni11 O103 C126 C121 59.4(2) . . . . ? C124 C125 C126 O103 177.9(2) . . . . ? C124 C125 C126 C121 -1.3(3) . . . . ? C122 C121 C126 O103 -179.5(2) . . . . ? C120 C121 C126 O103 -1.0(3) . . . . ? C122 C121 C126 C125 -0.3(3) . . . . ? C120 C121 C126 C125 178.1(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O102 H2 O1S 0.99(4) 1.50(4) 2.483(2) 171(3) . O1W H1WA O11 0.89(3) 1.83(3) 2.674(2) 159(3) . O1W H1WB O13 0.74(3) 1.98(3) 2.720(2) 176(3) 3_657 O1S H1S O101 0.87(4) 1.70(4) 2.569(2) 175(3) . _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.453 _refine_diff_density_min -0.445 _refine_diff_density_rms 0.080 #END data_5.2.5H2O.0.25MeOH3MeCN _database_code_depnum_ccdc_archive 'CCDC 606603' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H32 N4 Ni2 O8, 2.5(H2 O), C2 H3 N, 0.25(C H4 O)' _chemical_formula_sum 'C32.25 H41 N5 Ni2 O10.75' _chemical_formula_weight 788.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 44.353(5) _cell_length_b 8.850(5) _cell_length_c 19.517(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 112.433(5) _cell_angle_gamma 90.000(5) _cell_volume 7081(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3022 _cell_measurement_theta_max 38.699 _cell_measurement_theta_min 4.709 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.479 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3292 _exptl_absorpt_coefficient_mu 1.128 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5719 _exptl_absorpt_correction_T_max 0.7500 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ?5 _diffrn_reflns_number 35842 _diffrn_reflns_av_R_equivalents 0.0976 _diffrn_reflns_av_sigmaI/netI 0.0734 _diffrn_reflns_limit_h_min -53 _diffrn_reflns_limit_h_max 53 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6581 _reflns_number_gt 4443 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER Smart' _computing_cell_refinement 'BRUKER Smart' _computing_data_reduction ? _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0781P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6581 _refine_ls_number_parameters 466 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0921 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1520 _refine_ls_wR_factor_gt 0.1338 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni11 Ni 0.138531(13) 0.44015(6) 0.49597(3) 0.03759(18) Uani 1 1 d . . . Ni12 Ni 0.099244(13) 0.30704(6) 0.58338(3) 0.03766(18) Uani 1 1 d . . . O101 O 0.13263(8) 0.2946(3) 0.41186(17) 0.0489(8) Uani 1 1 d . . . O102 O 0.08188(9) 0.1050(4) 0.5306(2) 0.0558(10) Uani 1 1 d . . . O103 O 0.14133(7) 0.2635(3) 0.56893(15) 0.0377(7) Uani 1 1 d . . . N101 N 0.18588(9) 0.4620(4) 0.5159(2) 0.0417(9) Uani 1 1 d . . . N102 N 0.10412(9) 0.1962(4) 0.6772(2) 0.0436(9) Uani 1 1 d . . . N103 N 0.15136(8) 0.5924(4) 0.59444(19) 0.0392(9) Uani 1 1 d . . . N104 N 0.12127(8) 0.4893(4) 0.65672(19) 0.0391(9) Uani 1 1 d . . . O12W O 0.05270(9) 0.3688(5) 0.5727(3) 0.0594(10) Uani 1 1 d . . . O10 O 0.09108(7) 0.4220(3) 0.48595(16) 0.0404(7) Uani 1 1 d . . . O12 O 0.12482(8) 0.6319(4) 0.42932(18) 0.0507(8) Uani 1 1 d . . . C10 C 0.06537(11) 0.4676(5) 0.4316(3) 0.0439(11) Uani 1 1 d . . . O11 O 0.03769(8) 0.4615(4) 0.43213(19) 0.0635(10) Uani 1 1 d . . . C11 C 0.07125(12) 0.5293(6) 0.3655(2) 0.0525(13) Uani 1 1 d . . . H11G H 0.0507 0.5638 0.3286 0.063 Uiso 1 1 calc R . . H11H H 0.0795 0.4491 0.3436 0.063 Uiso 1 1 calc R . . C12 C 0.09572(13) 0.6610(5) 0.3871(3) 0.0469(12) Uani 1 1 d . . . O13 O 0.08522(9) 0.7882(4) 0.3616(2) 0.0633(10) Uani 1 1 d . . . C100 C 0.15418(12) 0.2588(5) 0.3840(2) 0.0443(11) Uani 1 1 d . . . C101 C 0.14515(14) 0.1642(5) 0.3205(3) 0.0533(13) Uani 1 1 d . . . H101 H 0.1238 0.1296 0.2996 0.064 Uiso 1 1 calc R . . C102 C 0.16652(16) 0.1213(6) 0.2885(3) 0.0628(15) Uani 1 1 d . . . H102 H 0.1594 0.0581 0.2474 0.075 Uiso 1 1 calc R . . C103 C 0.19836(16) 0.1712(6) 0.3168(3) 0.0663(16) Uani 1 1 d . . . H103 H 0.2128 0.1426 0.2949 0.080 Uiso 1 1 calc R . . C104 C 0.20848(13) 0.2644(6) 0.3783(3) 0.0571(13) Uani 1 1 d . . . H104 H 0.2300 0.2980 0.3977 0.069 Uiso 1 1 calc R . . C105 C 0.18721(12) 0.3096(5) 0.4123(3) 0.0476(12) Uani 1 1 d . . . C106 C 0.20088(12) 0.4056(5) 0.4772(3) 0.0474(12) Uani 1 1 d . . . H106 H 0.2229 0.4286 0.4924 0.057 Uiso 1 1 calc R . . C107 C 0.20468(11) 0.5536(5) 0.5808(3) 0.0474(12) Uani 1 1 d . . . H10A H 0.2219 0.6071 0.5720 0.057 Uiso 1 1 calc R . . H10B H 0.2145 0.4891 0.6238 0.057 Uiso 1 1 calc R . . C108 C 0.18150(12) 0.6667(5) 0.5949(3) 0.0505(12) Uani 1 1 d . . . H10C H 0.1926 0.7152 0.6425 0.061 Uiso 1 1 calc R . . H10D H 0.1756 0.7443 0.5569 0.061 Uiso 1 1 calc R . . C109 C 0.12615(12) 0.7098(5) 0.5890(3) 0.0514(12) Uani 1 1 d . . . H10E H 0.1128 0.7316 0.5376 0.062 Uiso 1 1 calc R . . H10F H 0.1364 0.8027 0.6132 0.062 Uiso 1 1 calc R . . C110 C 0.10561(12) 0.6399(5) 0.6286(3) 0.0512(13) Uani 1 1 d . . . H11A H 0.1059 0.7035 0.6693 0.061 Uiso 1 1 calc R . . H11B H 0.0832 0.6267 0.5944 0.061 Uiso 1 1 calc R . . C111 C 0.11783(12) 0.4479(5) 0.7278(3) 0.0494(12) Uani 1 1 d . . . H11C H 0.0961 0.4735 0.7246 0.059 Uiso 1 1 calc R . . H11D H 0.1333 0.5055 0.7682 0.059 Uiso 1 1 calc R . . C112 C 0.12383(12) 0.2793(6) 0.7437(2) 0.0508(12) Uani 1 1 d . . . H11E H 0.1467 0.2563 0.7569 0.061 Uiso 1 1 calc R . . H11F H 0.1178 0.2505 0.7848 0.061 Uiso 1 1 calc R . . C113 C 0.08515(12) 0.0897(5) 0.6817(3) 0.0468(12) Uani 1 1 d . . . H113 H 0.0850 0.0696 0.7284 0.056 Uiso 1 1 calc R . . C114 C 0.06402(11) -0.0016(5) 0.6205(3) 0.0482(12) Uani 1 1 d . . . C115 C 0.04348(13) -0.1052(6) 0.6360(3) 0.0616(14) Uani 1 1 d . . . H115 H 0.0439 -0.1119 0.6840 0.074 Uiso 1 1 calc R . . C116 C 0.02266(14) -0.1970(6) 0.5814(4) 0.0778(19) Uani 1 1 d . . . H116 H 0.0089 -0.2636 0.5923 0.093 Uiso 1 1 calc R . . C117 C 0.02231(14) -0.1897(6) 0.5110(4) 0.0742(17) Uani 1 1 d . . . H117 H 0.0083 -0.2521 0.4743 0.089 Uiso 1 1 calc R . . C118 C 0.04221(12) -0.0925(6) 0.4938(3) 0.0612(14) Uani 1 1 d . . . H118 H 0.0421 -0.0913 0.4461 0.073 Uiso 1 1 calc R . . C119 C 0.06267(11) 0.0048(5) 0.5471(3) 0.0487(12) Uani 1 1 d . . . C120 C 0.15584(10) 0.5164(5) 0.6662(2) 0.0408(11) Uani 1 1 d . . . H120 H 0.1656 0.5888 0.7066 0.049 Uiso 1 1 calc R . . C121 C 0.17705(10) 0.3770(5) 0.6822(2) 0.0390(10) Uani 1 1 d . . . C122 C 0.20497(11) 0.3697(6) 0.7458(3) 0.0512(12) Uani 1 1 d . . . H122 H 0.2098 0.4473 0.7805 0.061 Uiso 1 1 calc R . . C123 C 0.22568(12) 0.2482(6) 0.7581(3) 0.0601(14) Uani 1 1 d . . . H123 H 0.2444 0.2433 0.8011 0.072 Uiso 1 1 calc R . . C124 C 0.21866(13) 0.1340(6) 0.7067(3) 0.0616(15) Uani 1 1 d . . . H124 H 0.2330 0.0529 0.7150 0.074 Uiso 1 1 calc R . . C125 C 0.19048(12) 0.1377(5) 0.6426(3) 0.0500(12) Uani 1 1 d . . . H125 H 0.1861 0.0599 0.6081 0.060 Uiso 1 1 calc R . . C126 C 0.16892(10) 0.2577(5) 0.6302(2) 0.0385(10) Uani 1 1 d . . . H2 H 0.0838(12) 0.092(6) 0.497(3) 0.038(16) Uiso 1 1 d . . . H12A H 0.0411(12) 0.384(6) 0.601(3) 0.057(16) Uiso 1 1 d . . . H12B H 0.048(2) 0.381(10) 0.533(4) 0.14(4) Uiso 1 1 d . . . N1S N 0.23375(17) 0.9162(7) 0.5464(4) 0.104(2) Uani 1 1 d . . . C10S C 0.21533(17) 0.8794(8) 0.4916(5) 0.0775(19) Uani 1 1 d . . . C11S C 0.19170(19) 0.8246(9) 0.4208(4) 0.108(3) Uani 1 1 d . . . H11I H 0.1865 0.9042 0.3848 0.163 Uiso 1 1 calc R . . H11J H 0.1722 0.7929 0.4271 0.163 Uiso 1 1 calc R . . H11K H 0.2008 0.7407 0.4042 0.163 Uiso 1 1 calc R . . O1W O 0.08681(11) 0.0834(4) 0.4054(2) 0.0815(13) Uani 1 1 d . . . H1WA H 0.1057 0.1370 0.4055 0.100 Uiso 1 1 d . . . H1WB H 0.0961 -0.0194 0.3931 0.100 Uiso 1 1 d . . . O2W O 0.02052(10) 0.4056(6) 0.6641(2) 0.0950(15) Uani 1 1 d . . . H2W1 H 0.0193 0.3412 0.6985 0.100 Uiso 1 1 d . . . H2W2 H 0.0028 0.4442 0.6354 0.100 Uiso 1 1 d . . . O3W O 0.0166(2) 0.8026(12) 0.2700(5) 0.077(3) Uiso 0.40 1 d P A 1 O3W' O 0.0000 0.920(3) 0.2500 0.074(8) Uiso 0.20 2 d SP B 2 O2S O 0.0175(6) 1.087(3) 0.2859(13) 0.141(9) Uiso 0.25 1 d PD C 3 H2S H 0.0362 1.1040 0.3151 0.212 Uiso 0.25 1 calc PR C 3 C2S C 0.0000 1.242(3) 0.2500 0.155(10) Uiso 0.50 2 d SPD C 3 H2S1 H -0.0162 1.2673 0.2697 0.233 Uiso 0.25 1 calc PR C 3 H2S2 H -0.0102 1.2314 0.1972 0.233 Uiso 0.25 1 calc PR C 3 H2S3 H 0.0160 1.3217 0.2617 0.233 Uiso 0.25 1 calc PR C 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni11 0.0399(3) 0.0318(3) 0.0413(3) -0.0023(2) 0.0158(3) -0.0048(2) Ni12 0.0408(3) 0.0337(3) 0.0391(3) -0.0015(2) 0.0160(2) -0.0040(3) O101 0.0501(19) 0.048(2) 0.0522(19) -0.0096(16) 0.0232(16) -0.0072(16) O102 0.072(3) 0.048(2) 0.057(2) -0.0127(19) 0.036(2) -0.0248(18) O103 0.0418(17) 0.0298(16) 0.0410(16) 0.0000(13) 0.0153(14) -0.0020(13) N101 0.045(2) 0.034(2) 0.050(2) -0.0025(18) 0.0219(18) -0.0026(17) N102 0.047(2) 0.042(2) 0.042(2) 0.0012(18) 0.0176(18) 0.0017(18) N103 0.040(2) 0.031(2) 0.045(2) -0.0026(16) 0.0145(17) -0.0021(16) N104 0.040(2) 0.034(2) 0.045(2) -0.0041(17) 0.0176(17) -0.0002(17) O12W 0.046(2) 0.078(3) 0.059(3) 0.011(2) 0.025(2) 0.0030(19) O10 0.0372(16) 0.0383(17) 0.0421(17) 0.0009(14) 0.0112(14) -0.0015(13) O12 0.052(2) 0.0440(19) 0.0533(19) 0.0075(16) 0.0169(17) -0.0092(16) C10 0.042(3) 0.036(3) 0.049(3) -0.002(2) 0.012(2) -0.006(2) O11 0.040(2) 0.082(3) 0.065(2) 0.020(2) 0.0154(17) 0.0008(18) C11 0.055(3) 0.058(3) 0.040(3) 0.008(2) 0.013(2) -0.003(3) C12 0.061(3) 0.043(3) 0.042(3) 0.000(2) 0.026(2) 0.001(2) O13 0.087(3) 0.040(2) 0.067(2) 0.0116(18) 0.035(2) 0.0125(19) C100 0.060(3) 0.030(2) 0.046(3) 0.008(2) 0.024(2) 0.000(2) C101 0.077(4) 0.038(3) 0.045(3) 0.001(2) 0.024(3) 0.001(3) C102 0.105(5) 0.043(3) 0.051(3) 0.001(2) 0.040(3) 0.008(3) C103 0.089(5) 0.052(3) 0.078(4) 0.008(3) 0.054(4) 0.017(3) C104 0.067(3) 0.046(3) 0.069(4) 0.000(3) 0.038(3) 0.005(3) C105 0.058(3) 0.041(3) 0.048(3) 0.001(2) 0.025(2) 0.003(2) C106 0.044(3) 0.043(3) 0.056(3) 0.000(2) 0.021(2) -0.005(2) C107 0.045(3) 0.044(3) 0.051(3) -0.006(2) 0.015(2) -0.010(2) C108 0.054(3) 0.038(3) 0.060(3) -0.009(2) 0.023(2) -0.019(2) C109 0.063(3) 0.034(3) 0.059(3) -0.005(2) 0.025(3) 0.003(2) C110 0.054(3) 0.037(3) 0.060(3) -0.010(2) 0.018(2) 0.009(2) C111 0.056(3) 0.053(3) 0.045(3) -0.011(2) 0.025(2) -0.005(2) C112 0.057(3) 0.058(3) 0.041(3) 0.000(2) 0.022(2) -0.004(2) C113 0.056(3) 0.038(3) 0.055(3) 0.011(2) 0.030(2) 0.007(2) C114 0.040(3) 0.039(3) 0.070(3) 0.006(2) 0.026(2) 0.002(2) C115 0.067(4) 0.043(3) 0.087(4) 0.006(3) 0.043(3) -0.001(3) C116 0.064(4) 0.051(4) 0.128(6) -0.002(4) 0.047(4) -0.019(3) C117 0.069(4) 0.055(4) 0.100(5) -0.023(3) 0.034(4) -0.024(3) C118 0.054(3) 0.049(3) 0.076(4) -0.013(3) 0.019(3) -0.009(3) C119 0.046(3) 0.031(2) 0.071(3) -0.003(2) 0.024(2) -0.002(2) C120 0.042(3) 0.034(2) 0.043(3) -0.007(2) 0.012(2) -0.003(2) C121 0.040(3) 0.036(2) 0.041(2) -0.001(2) 0.016(2) -0.002(2) C122 0.044(3) 0.051(3) 0.054(3) 0.006(2) 0.013(2) 0.002(2) C123 0.049(3) 0.062(4) 0.063(3) 0.018(3) 0.014(3) 0.004(3) C124 0.053(3) 0.053(3) 0.081(4) 0.022(3) 0.028(3) 0.018(3) C125 0.053(3) 0.036(3) 0.063(3) 0.005(2) 0.024(3) 0.005(2) C126 0.038(2) 0.031(2) 0.049(3) 0.005(2) 0.019(2) -0.001(2) N1S 0.105(5) 0.100(5) 0.111(5) -0.007(4) 0.045(4) -0.036(4) C10S 0.074(5) 0.066(4) 0.105(6) 0.017(4) 0.048(4) -0.008(4) C11S 0.112(6) 0.115(6) 0.088(5) 0.040(5) 0.027(5) -0.014(5) O1W 0.109(3) 0.062(3) 0.097(3) -0.028(2) 0.066(3) -0.031(2) O2W 0.079(3) 0.136(4) 0.070(3) 0.023(3) 0.029(2) 0.023(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni11 N101 1.994(4) . ? Ni11 O101 2.024(3) . ? Ni11 O10 2.044(3) . ? Ni11 O12 2.083(3) . ? Ni11 O103 2.086(3) . ? Ni11 N103 2.236(4) . ? Ni12 N102 2.016(4) . ? Ni12 O103 2.028(3) . ? Ni12 O102 2.061(4) . ? Ni12 O10 2.063(3) . ? Ni12 O12W 2.067(4) . ? Ni12 N104 2.130(4) . ? O101 C100 1.306(5) . ? O102 C119 1.351(6) . ? O102 H2 0.69(4) . ? O103 C126 1.346(5) . ? N101 C106 1.282(6) . ? N101 C107 1.467(5) . ? N102 C113 1.288(6) . ? N102 C112 1.457(6) . ? N103 C108 1.487(6) . ? N103 C120 1.497(5) . ? N103 C109 1.501(6) . ? N104 C120 1.492(5) . ? N104 C111 1.498(6) . ? N104 C110 1.506(6) . ? O12W H12A 0.90(5) . ? O12W H12B 0.73(8) . ? O10 C10 1.290(5) . ? O11 C10 1.233(5) . ? O12 C12 1.265(5) . ? O13 C12 1.247(5) . ? C10 C11 1.513(6) . ? C11 C12 1.538(7) . ? C11 H11G 0.9700 . ? C11 H11H 0.9700 . ? C100 C101 1.421(6) . ? C100 C105 1.427(7) . ? C101 C102 1.372(7) . ? C101 H101 0.9300 . ? C102 C103 1.378(8) . ? C102 H102 0.9300 . ? C103 C104 1.383(7) . ? C103 H103 0.9300 . ? C104 C105 1.402(6) . ? C104 H104 0.9300 . ? C105 C106 1.452(6) . ? C106 H106 0.9300 . ? C107 C108 1.533(6) . ? C107 H10A 0.9700 . ? C107 H10B 0.9700 . ? C108 H10C 0.9700 . ? C108 H10D 0.9700 . ? C109 C110 1.531(7) . ? C109 H10E 0.9700 . ? C109 H10F 0.9700 . ? C110 H11A 0.9700 . ? C110 H11B 0.9700 . ? C111 C112 1.527(7) . ? C111 H11C 0.9700 . ? C111 H11D 0.9700 . ? C112 H11E 0.9700 . ? C112 H11F 0.9700 . ? C113 C114 1.451(7) . ? C113 H113 0.9300 . ? C114 C115 1.404(7) . ? C114 C119 1.413(7) . ? C115 C116 1.378(8) . ? C115 H115 0.9300 . ? C116 C117 1.371(9) . ? C116 H116 0.9300 . ? C117 C118 1.363(7) . ? C117 H117 0.9300 . ? C118 C119 1.388(7) . ? C118 H118 0.9300 . ? C120 C121 1.510(6) . ? C120 H120 0.9800 . ? C121 C122 1.381(6) . ? C121 C126 1.412(6) . ? C122 C123 1.375(7) . ? C122 H122 0.9300 . ? C123 C124 1.373(7) . ? C123 H123 0.9300 . ? C124 C125 1.392(7) . ? C124 H124 0.9300 . ? C125 C126 1.387(6) . ? C125 H125 0.9300 . ? N1S C10S 1.119(8) . ? C10S C11S 1.461(10) . ? C11S H11I 0.9600 . ? C11S H11J 0.9600 . ? C11S H11K 0.9600 . ? O1W H1WA 0.9614 . ? O1W H1WB 1.0630 . ? O2W H2W1 0.8988 . ? O2W H2W2 0.8428 . ? O2S C2S 1.61(3) . ? O2S H2S 0.8200 . ? C2S H2S1 0.9600 . ? C2S H2S2 0.9600 . ? C2S H2S3 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N101 Ni11 O101 91.17(14) . . ? N101 Ni11 O10 174.58(13) . . ? O101 Ni11 O10 93.59(12) . . ? N101 Ni11 O12 94.44(13) . . ? O101 Ni11 O12 95.48(13) . . ? O10 Ni11 O12 87.69(12) . . ? N101 Ni11 O103 98.97(13) . . ? O101 Ni11 O103 91.84(13) . . ? O10 Ni11 O103 78.30(11) . . ? O12 Ni11 O103 164.58(12) . . ? N101 Ni11 N103 82.56(14) . . ? O101 Ni11 N103 173.09(13) . . ? O10 Ni11 N103 92.56(12) . . ? O12 Ni11 N103 87.93(13) . . ? O103 Ni11 N103 86.30(13) . . ? N102 Ni12 O103 104.40(13) . . ? N102 Ni12 O102 85.52(16) . . ? O103 Ni12 O102 87.36(14) . . ? N102 Ni12 O10 176.29(13) . . ? O103 Ni12 O10 79.20(11) . . ? O102 Ni12 O10 93.80(14) . . ? N102 Ni12 O12W 88.70(17) . . ? O103 Ni12 O12W 166.52(15) . . ? O102 Ni12 O12W 90.59(17) . . ? O10 Ni12 O12W 87.65(15) . . ? N102 Ni12 N104 84.00(15) . . ? O103 Ni12 N104 91.54(12) . . ? O102 Ni12 N104 168.84(15) . . ? O10 Ni12 N104 96.90(13) . . ? O12W Ni12 N104 92.98(16) . . ? C100 O101 Ni11 127.1(3) . . ? C119 O102 Ni12 126.9(3) . . ? C119 O102 H2 115(4) . . ? Ni12 O102 H2 117(4) . . ? C126 O103 Ni12 117.2(2) . . ? C126 O103 Ni11 115.6(2) . . ? Ni12 O103 Ni11 97.72(12) . . ? C106 N101 C107 118.2(4) . . ? C106 N101 Ni11 126.3(3) . . ? C107 N101 Ni11 115.5(3) . . ? C113 N102 C112 119.6(4) . . ? C113 N102 Ni12 124.9(3) . . ? C112 N102 Ni12 112.5(3) . . ? C108 N103 C120 113.3(3) . . ? C108 N103 C109 109.8(3) . . ? C120 N103 C109 101.9(3) . . ? C108 N103 Ni11 101.8(3) . . ? C120 N103 Ni11 115.7(3) . . ? C109 N103 Ni11 114.7(3) . . ? C120 N104 C111 112.8(3) . . ? C120 N104 C110 102.3(3) . . ? C111 N104 C110 111.0(3) . . ? C120 N104 Ni12 113.0(3) . . ? C111 N104 Ni12 104.7(3) . . ? C110 N104 Ni12 113.3(3) . . ? Ni12 O12W H12A 140(3) . . ? Ni12 O12W H12B 91(7) . . ? H12A O12W H12B 129(7) . . ? C10 O10 Ni11 127.5(3) . . ? C10 O10 Ni12 134.5(3) . . ? Ni11 O10 Ni12 97.96(12) . . ? C12 O12 Ni11 123.7(3) . . ? O11 C10 O10 123.4(4) . . ? O11 C10 C11 121.3(4) . . ? O10 C10 C11 115.3(4) . . ? C10 C11 C12 111.9(4) . . ? C10 C11 H11G 109.2 . . ? C12 C11 H11G 109.2 . . ? C10 C11 H11H 109.2 . . ? C12 C11 H11H 109.2 . . ? H11G C11 H11H 107.9 . . ? O13 C12 O12 125.2(5) . . ? O13 C12 C11 117.3(5) . . ? O12 C12 C11 117.5(4) . . ? O101 C100 C101 119.9(4) . . ? O101 C100 C105 124.7(4) . . ? C101 C100 C105 115.4(4) . . ? C102 C101 C100 123.1(5) . . ? C102 C101 H101 118.5 . . ? C100 C101 H101 118.5 . . ? C101 C102 C103 120.6(5) . . ? C101 C102 H102 119.7 . . ? C103 C102 H102 119.7 . . ? C102 C103 C104 118.8(5) . . ? C102 C103 H103 120.6 . . ? C104 C103 H103 120.6 . . ? C103 C104 C105 121.7(5) . . ? C103 C104 H104 119.1 . . ? C105 C104 H104 119.1 . . ? N101 C106 C105 127.2(4) . . ? N101 C106 H106 116.4 . . ? C105 C106 H106 116.4 . . ? C104 C105 C100 120.3(5) . . ? C104 C105 C106 116.6(5) . . ? C100 C105 C106 123.1(4) . . ? N101 C107 C108 108.4(4) . . ? N101 C107 H10A 110.0 . . ? C108 C107 H10A 110.0 . . ? N101 C107 H10B 110.0 . . ? C108 C107 H10B 110.0 . . ? H10A C107 H10B 108.4 . . ? N103 C108 C107 111.9(4) . . ? N103 C108 H10C 109.2 . . ? C107 C108 H10C 109.2 . . ? N103 C108 H10D 109.2 . . ? C107 C108 H10D 109.2 . . ? H10C C108 H10D 107.9 . . ? N103 C109 C110 104.8(4) . . ? N103 C109 H10E 110.8 . . ? C110 C109 H10E 110.8 . . ? N103 C109 H10F 110.8 . . ? C110 C109 H10F 110.8 . . ? H10E C109 H10F 108.9 . . ? N104 C110 C109 105.1(4) . . ? N104 C110 H11A 110.7 . . ? C109 C110 H11A 110.7 . . ? N104 C110 H11B 110.7 . . ? C109 C110 H11B 110.7 . . ? H11A C110 H11B 108.8 . . ? N104 C111 C112 110.8(4) . . ? N104 C111 H11C 109.5 . . ? C112 C111 H11C 109.5 . . ? N104 C111 H11D 109.5 . . ? C112 C111 H11D 109.5 . . ? H11C C111 H11D 108.1 . . ? N102 C112 C111 108.3(4) . . ? N102 C112 H11E 110.0 . . ? C111 C112 H11E 110.0 . . ? N102 C112 H11F 110.0 . . ? C111 C112 H11F 110.0 . . ? H11E C112 H11F 108.4 . . ? N102 C113 C114 125.8(4) . . ? N102 C113 H113 117.1 . . ? C114 C113 H113 117.1 . . ? C115 C114 C119 117.7(5) . . ? C115 C114 C113 117.0(5) . . ? C119 C114 C113 125.2(4) . . ? C116 C115 C114 121.1(6) . . ? C116 C115 H115 119.4 . . ? C114 C115 H115 119.4 . . ? C117 C116 C115 119.7(5) . . ? C117 C116 H116 120.1 . . ? C115 C116 H116 120.1 . . ? C118 C117 C116 121.0(6) . . ? C118 C117 H117 119.5 . . ? C116 C117 H117 119.5 . . ? C117 C118 C119 120.5(6) . . ? C117 C118 H118 119.7 . . ? C119 C118 H118 119.7 . . ? O102 C119 C118 121.4(5) . . ? O102 C119 C114 118.8(4) . . ? C118 C119 C114 119.8(5) . . ? N104 C120 N103 101.1(3) . . ? N104 C120 C121 115.1(4) . . ? N103 C120 C121 114.2(3) . . ? N104 C120 H120 108.7 . . ? N103 C120 H120 108.7 . . ? C121 C120 H120 108.7 . . ? C122 C121 C126 120.5(4) . . ? C122 C121 C120 119.9(4) . . ? C126 C121 C120 119.6(4) . . ? C123 C122 C121 120.2(5) . . ? C123 C122 H122 119.9 . . ? C121 C122 H122 119.9 . . ? C124 C123 C122 119.9(5) . . ? C124 C123 H123 120.1 . . ? C122 C123 H123 120.1 . . ? C123 C124 C125 121.0(5) . . ? C123 C124 H124 119.5 . . ? C125 C124 H124 119.5 . . ? C126 C125 C124 119.8(5) . . ? C126 C125 H125 120.1 . . ? C124 C125 H125 120.1 . . ? O103 C126 C125 121.1(4) . . ? O103 C126 C121 120.4(4) . . ? C125 C126 C121 118.5(4) . . ? N1S C10S C11S 177.5(9) . . ? C10S C11S H11I 109.5 . . ? C10S C11S H11J 109.5 . . ? H11I C11S H11J 109.5 . . ? C10S C11S H11K 109.5 . . ? H11I C11S H11K 109.5 . . ? H11J C11S H11K 109.5 . . ? H1WA O1W H1WB 90.6 . . ? H2W1 O2W H2W2 116.6 . . ? C2S O2S H2S 109.5 . . ? O2S C2S H2S1 109.5 . . ? O2S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? O2S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N101 Ni11 O101 C100 -7.1(4) . . . . ? O10 Ni11 O101 C100 175.5(3) . . . . ? O12 Ni11 O101 C100 87.5(4) . . . . ? O103 Ni11 O101 C100 -106.1(4) . . . . ? N102 Ni12 O102 C119 37.8(4) . . . . ? O103 Ni12 O102 C119 142.4(4) . . . . ? O10 Ni12 O102 C119 -138.6(4) . . . . ? O12W Ni12 O102 C119 -50.9(4) . . . . ? N104 Ni12 O102 C119 57.9(10) . . . . ? N102 Ni12 O103 C126 -37.4(3) . . . . ? O102 Ni12 O103 C126 -122.0(3) . . . . ? O10 Ni12 O103 C126 143.6(3) . . . . ? O12W Ni12 O103 C126 156.5(6) . . . . ? N104 Ni12 O103 C126 46.9(3) . . . . ? N102 Ni12 O103 Ni11 -161.38(13) . . . . ? O102 Ni12 O103 Ni11 113.94(15) . . . . ? O10 Ni12 O103 Ni11 19.56(11) . . . . ? O12W Ni12 O103 Ni11 32.4(7) . . . . ? N104 Ni12 O103 Ni11 -77.17(14) . . . . ? N101 Ni11 O103 C126 30.3(3) . . . . ? O101 Ni11 O103 C126 121.8(3) . . . . ? O10 Ni11 O103 C126 -145.0(3) . . . . ? O12 Ni11 O103 C126 -119.8(5) . . . . ? N103 Ni11 O103 C126 -51.6(3) . . . . ? N101 Ni11 O103 Ni12 155.44(13) . . . . ? O101 Ni11 O103 Ni12 -113.09(13) . . . . ? O10 Ni11 O103 Ni12 -19.81(11) . . . . ? O12 Ni11 O103 Ni12 5.3(5) . . . . ? N103 Ni11 O103 Ni12 73.58(13) . . . . ? O101 Ni11 N101 C106 5.8(4) . . . . ? O12 Ni11 N101 C106 -89.8(4) . . . . ? O103 Ni11 N101 C106 97.8(4) . . . . ? N103 Ni11 N101 C106 -177.2(4) . . . . ? O101 Ni11 N101 C107 -175.0(3) . . . . ? O12 Ni11 N101 C107 89.4(3) . . . . ? O103 Ni11 N101 C107 -82.9(3) . . . . ? N103 Ni11 N101 C107 2.1(3) . . . . ? O103 Ni12 N102 C113 -119.2(4) . . . . ? O102 Ni12 N102 C113 -33.1(4) . . . . ? O12W Ni12 N102 C113 57.6(4) . . . . ? N104 Ni12 N102 C113 150.7(4) . . . . ? O103 Ni12 N102 C112 80.5(3) . . . . ? O102 Ni12 N102 C112 166.7(3) . . . . ? O12W Ni12 N102 C112 -102.6(3) . . . . ? N104 Ni12 N102 C112 -9.5(3) . . . . ? N101 Ni11 N103 C108 22.7(3) . . . . ? O10 Ni11 N103 C108 -159.6(3) . . . . ? O12 Ni11 N103 C108 -72.0(3) . . . . ? O103 Ni11 N103 C108 122.3(3) . . . . ? N101 Ni11 N103 C120 -100.5(3) . . . . ? O10 Ni11 N103 C120 77.1(3) . . . . ? O12 Ni11 N103 C120 164.7(3) . . . . ? O103 Ni11 N103 C120 -1.0(3) . . . . ? N101 Ni11 N103 C109 141.2(3) . . . . ? O10 Ni11 N103 C109 -41.1(3) . . . . ? O12 Ni11 N103 C109 46.5(3) . . . . ? O103 Ni11 N103 C109 -119.2(3) . . . . ? N102 Ni12 N104 C120 106.3(3) . . . . ? O103 Ni12 N104 C120 2.0(3) . . . . ? O102 Ni12 N104 C120 86.2(8) . . . . ? O10 Ni12 N104 C120 -77.3(3) . . . . ? O12W Ni12 N104 C120 -165.3(3) . . . . ? N102 Ni12 N104 C111 -16.8(3) . . . . ? O103 Ni12 N104 C111 -121.1(3) . . . . ? O102 Ni12 N104 C111 -37.0(9) . . . . ? O10 Ni12 N104 C111 159.6(3) . . . . ? O12W Ni12 N104 C111 71.6(3) . . . . ? N102 Ni12 N104 C110 -137.9(3) . . . . ? O103 Ni12 N104 C110 117.7(3) . . . . ? O102 Ni12 N104 C110 -158.1(7) . . . . ? O10 Ni12 N104 C110 38.4(3) . . . . ? O12W Ni12 N104 C110 -49.6(3) . . . . ? O101 Ni11 O10 C10 -67.3(4) . . . . ? O12 Ni11 O10 C10 28.1(3) . . . . ? O103 Ni11 O10 C10 -158.4(4) . . . . ? N103 Ni11 O10 C10 115.9(3) . . . . ? O101 Ni11 O10 Ni12 110.62(13) . . . . ? O12 Ni11 O10 Ni12 -154.03(13) . . . . ? O103 Ni11 O10 Ni12 19.47(11) . . . . ? N103 Ni11 O10 Ni12 -66.21(14) . . . . ? O103 Ni12 O10 C10 157.7(4) . . . . ? O102 Ni12 O10 C10 71.1(4) . . . . ? O12W Ni12 O10 C10 -19.3(4) . . . . ? N104 Ni12 O10 C10 -112.1(4) . . . . ? O103 Ni12 O10 Ni11 -19.98(11) . . . . ? O102 Ni12 O10 Ni11 -106.56(14) . . . . ? O12W Ni12 O10 Ni11 163.00(16) . . . . ? N104 Ni12 O10 Ni11 70.28(14) . . . . ? N101 Ni11 O12 C12 165.0(4) . . . . ? O101 Ni11 O12 C12 73.4(4) . . . . ? O10 Ni11 O12 C12 -19.9(4) . . . . ? O103 Ni11 O12 C12 -44.6(7) . . . . ? N103 Ni11 O12 C12 -112.6(4) . . . . ? Ni11 O10 C10 O11 -174.8(3) . . . . ? Ni12 O10 C10 O11 8.1(7) . . . . ? Ni11 O10 C10 C11 5.5(6) . . . . ? Ni12 O10 C10 C11 -171.5(3) . . . . ? O11 C10 C11 C12 123.5(5) . . . . ? O10 C10 C11 C12 -56.9(6) . . . . ? Ni11 O12 C12 O13 160.4(4) . . . . ? Ni11 O12 C12 C11 -19.4(6) . . . . ? C10 C11 C12 O13 -114.0(5) . . . . ? C10 C11 C12 O12 65.8(6) . . . . ? Ni11 O101 C100 C101 -174.5(3) . . . . ? Ni11 O101 C100 C105 4.7(6) . . . . ? O101 C100 C101 C102 -179.7(4) . . . . ? C105 C100 C101 C102 1.0(7) . . . . ? C100 C101 C102 C103 -0.8(8) . . . . ? C101 C102 C103 C104 0.4(8) . . . . ? C102 C103 C104 C105 -0.2(8) . . . . ? C107 N101 C106 C105 178.5(4) . . . . ? Ni11 N101 C106 C105 -2.2(7) . . . . ? C103 C104 C105 C100 0.5(7) . . . . ? C103 C104 C105 C106 179.0(5) . . . . ? O101 C100 C105 C104 179.9(4) . . . . ? C101 C100 C105 C104 -0.8(6) . . . . ? O101 C100 C105 C106 1.4(7) . . . . ? C101 C100 C105 C106 -179.3(4) . . . . ? N101 C106 C105 C104 178.6(5) . . . . ? N101 C106 C105 C100 -2.8(8) . . . . ? C106 N101 C107 C108 152.9(4) . . . . ? Ni11 N101 C107 C108 -26.4(5) . . . . ? C120 N103 C108 C107 81.1(5) . . . . ? C109 N103 C108 C107 -165.8(4) . . . . ? Ni11 N103 C108 C107 -43.8(4) . . . . ? N101 C107 C108 N103 48.7(5) . . . . ? C108 N103 C109 C110 -151.0(4) . . . . ? C120 N103 C109 C110 -30.7(4) . . . . ? Ni11 N103 C109 C110 95.1(4) . . . . ? C120 N104 C110 C109 27.2(4) . . . . ? C111 N104 C110 C109 147.8(4) . . . . ? Ni12 N104 C110 C109 -94.7(4) . . . . ? N103 C109 C110 N104 2.2(5) . . . . ? C120 N104 C111 C112 -83.5(4) . . . . ? C110 N104 C111 C112 162.4(4) . . . . ? Ni12 N104 C111 C112 39.8(4) . . . . ? C113 N102 C112 C111 -127.8(4) . . . . ? Ni12 N102 C112 C111 33.6(4) . . . . ? N104 C111 C112 N102 -49.7(5) . . . . ? C112 N102 C113 C114 179.5(4) . . . . ? Ni12 N102 C113 C114 20.6(7) . . . . ? N102 C113 C114 C115 -175.7(5) . . . . ? N102 C113 C114 C119 4.8(8) . . . . ? C119 C114 C115 C116 -0.2(8) . . . . ? C113 C114 C115 C116 -179.8(5) . . . . ? C114 C115 C116 C117 1.3(9) . . . . ? C115 C116 C117 C118 -0.2(10) . . . . ? C116 C117 C118 C119 -1.9(9) . . . . ? Ni12 O102 C119 C118 153.9(4) . . . . ? Ni12 O102 C119 C114 -27.1(6) . . . . ? C117 C118 C119 O102 -178.1(5) . . . . ? C117 C118 C119 C114 2.9(8) . . . . ? C115 C114 C119 O102 179.1(4) . . . . ? C113 C114 C119 O102 -1.4(7) . . . . ? C115 C114 C119 C118 -1.8(7) . . . . ? C113 C114 C119 C118 177.7(5) . . . . ? C111 N104 C120 N103 -166.0(3) . . . . ? C110 N104 C120 N103 -46.7(4) . . . . ? Ni12 N104 C120 N103 75.5(3) . . . . ? C111 N104 C120 C121 70.4(5) . . . . ? C110 N104 C120 C121 -170.3(4) . . . . ? Ni12 N104 C120 C121 -48.2(4) . . . . ? C108 N103 C120 N104 166.0(3) . . . . ? C109 N103 C120 N104 48.2(4) . . . . ? Ni11 N103 C120 N104 -77.0(3) . . . . ? C108 N103 C120 C121 -69.8(5) . . . . ? C109 N103 C120 C121 172.4(4) . . . . ? Ni11 N103 C120 C121 47.2(4) . . . . ? N104 C120 C121 C122 -122.3(4) . . . . ? N103 C120 C121 C122 121.4(4) . . . . ? N104 C120 C121 C126 60.5(5) . . . . ? N103 C120 C121 C126 -55.8(5) . . . . ? C126 C121 C122 C123 2.0(7) . . . . ? C120 C121 C122 C123 -175.2(4) . . . . ? C121 C122 C123 C124 0.3(8) . . . . ? C122 C123 C124 C125 -1.1(8) . . . . ? C123 C124 C125 C126 -0.5(8) . . . . ? Ni12 O103 C126 C125 130.5(4) . . . . ? Ni11 O103 C126 C125 -115.1(4) . . . . ? Ni12 O103 C126 C121 -51.6(5) . . . . ? Ni11 O103 C126 C121 62.8(4) . . . . ? C124 C125 C126 O103 -179.4(4) . . . . ? C124 C125 C126 C121 2.7(7) . . . . ? C122 C121 C126 O103 178.6(4) . . . . ? C120 C121 C126 O103 -4.2(6) . . . . ? C122 C121 C126 C125 -3.5(6) . . . . ? C120 C121 C126 C125 173.7(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O102 H2 O1W 0.69(4) 1.85(5) 2.543(5) 172(6) . O12W H12A O2W 0.90(5) 1.80(5) 2.697(6) 175(5) . O12W H12B O11 0.73(8) 1.97(8) 2.692(6) 167(10) . O1W H1WA O101 0.96 1.81 2.728(5) 158.7 . O1W H1WB O13 1.06 1.81 2.741(5) 143.6 1_545 O2W H2W1 O3W 0.90 1.93 2.824(11) 178.0 6_566 O2W H2W2 O11 0.84 1.96 2.806(5) 178.4 5_566 O2S H2S O1W 0.82 2.27 3.07(2) 163.7 1_565 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.804 _refine_diff_density_min -0.441 _refine_diff_density_rms 0.081 #END